Materials Chemistry and Physics 227 (2019) 130–133

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Materials Chemistry and Physics

journal homepage: www.elsevier.com/locate/matchemphys

Sintering behavior and microwave dielectric properties of low-loss T

Li2Mg3TiO6 ceramics doped with different glass agents
Ping Zhanga,∗, Miaomiao Yanga, Hui Xiea, Mi Xiaoa, Zhentai Zhengb
a
School of Electrical and Information Engineering and Key Laboratory of Advanced Ceramics and Machining Technology of Ministry of Education, Tianjin University,
Tianjin, 300072, China
b
School of Materials Science and Engineering, Hebei University of Technology, Tianjin, 300130, China

H I GH L IG H T S

• The Li Mg TiO -xwt%ZBS/LBS were prepared by solid-state reaction method.

2 3 6

• The sintering temperature of Li Mg TiO ceramics reduced to 1025 °C from 1350 °C.
2 3 6

• Li Mg TiO -4wt%ZBS ceramics exhibited excellent dielectric properties.

2 3 6

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

Keywords: The Li2Mg3TiO6 ceramics doped with ZnOeB2O3eSiO2 (ZBS)/Li2OeB2O3eSiO2 (ZBS) glass were synthesized
Li2Mg3TiO6 through the conventional solid-state reaction route. The phase compositions, microstructures, sintering char-
Microwave dielectric properties acteristics and microwave dielectric properties of Li2Mg3TiO6-xwt%ZBS and Li2Mg3TiO6-xwt%LBS (0 ≤ x ≤ 8)
Sintering temperature were investigated. With the increase of low-melting ZBS/LBS glass, the densification of Li2Mg3TiO6 ceramics was
ZBS glass
improved significantly through the mechanism of liquid phase sintering. The addition of ZBS/LBS glass could
LBS glass
effectively lower the sintering temperature from 1350 °C to 1025 °C/1050 °C and had slightly influences on
microwave dielectric properties of Li2Mg3TiO6 ceramics. The dielectric constant ɛr and Q×f values correlated
with bulk density strongly. The temperature coefficient of resonant frequency (τf) was reduced by adding ZBS/
LBS glass, due to the formation of the second phase MgSiO4. Compared with Li2Mg3TiO6-4wt%LBS sintered at
1050 °C, Li2Mg3TiO6 ceramics with 4 wt% ZBS glass sintered at 1025 °C had higher densification and more
uniform grain morphology, which displayed excellent microwave dielectric properties of ɛr∼13.35,
Q×f∼138,800 GHz and τƒ∼-31.84 ppm/°C.

1. Introduction
With the increasing demands of low loss and light weighted devices
in wireless communication, microwave dielectric ceramics which have
high dielectric constant, high Q×f value and near-zero temperature
coefficient of resonant frequency have been widely concerned and ap-
plied in microwave devices such as filters, oscillator components and
transmission lines [1–3]. Moreover, these ceramics are also expected to
co-fire with a high conductive electrode such as Ag or Cu (melting point
961 °C and 1083 °C). Therefore, it is necessary to reduce the sintering
temperature of ceramics which have excellent microwave dielectric
properties [4–6].
Fu et al. have reported that Li2Mg3TiO6 have excellent microwave
dielectric properties (ɛr∼15.2, Q×f∼152,000 GHz and τƒ∼39 ppm/°C)
when sintered at 1280 °C for 6 h [7]. Afterwards, they also reported that
Li2Mg3TiO6 ceramics with 4 wt% LiF sintered at 950 °C possessed good
dielectric properties of ɛr = 16.2, Q×f = 131,000 GHz and
τƒ = −44 ppm/°C [8]. Recently, low-melting glasses such as MgOe-
B2O3eSiO2, ZnOeB2O3eSiO2 and Li2OeB2O3eSiO2 glass [9–12] were
used to lower the sintering temperature of ceramics. In previous re-
ports, the microwave dielectric properties of Li3Mg2NbO6 ceramics with
0.5 wt% ZBS glass addition sintered at 925 °C for 4 h are ɛr ∼14.84,
Q×f∼73,985 GHz and τƒ∼-16.07 ppm/°C, and the microwave di-
electric properties of Li3Mg2NbO6 ceramics with 1 wt% LBS glass sin-
tered at 875 °C are ɛr ∼14.84, Q×f∼73,985 GHz and τƒ∼-16.07 ppm/
°C [11,13]. The 0.6Li2ZnTi3O8-0.4Li2TiO3 ceramics with 1.0 wt% ZBS
glass could be well sintered at 900 °C with microwave dielectric prop-
erties of ɛr ∼25.4, Q×f∼86,400 GHz and τƒ∼-1.0 ppm/°C [12]. Wu

∗
Corresponding author.
E-mail address: zptai@163.com (P. Zhang).

https://doi.org/10.1016/j.matchemphys.2018.12.045
Received 10 October 2018; Received in revised form 29 November 2018; Accepted 15 December 2018
Available online 31 January 2019
0254-0584/ © 2019 Elsevier B.V. All rights reserved.
P. Zhang et al. Materials Chemistry and Physics 227 (2019) 130–133

et al. reported that ZnOeB2O3eSiO2 glass had a low softening tem-

perature of 581 °C [14]. It is speculated that ZnOeB2O3eSiO2 and
Li2OeB2O3eSiO2 glass may reduce the sintering temperature of some
lithium-based ceramics. Therefore, we have attempted to demonstrate a
comprehensive study of Li2Mg3TiO6 ceramics doped with different
amounts of ZBS and LBS glass.
In this work, we used xwt% (0 ≤ x ≤ 8) ZnOeB2O3eSiO2 (ZBS) and
Li2OeB2O3eSiO2 (LBS) glasses to lower the sintering temperature of
Li2Mg3TiO6 ceramics. And the phase compositions, sintering char-
acteristic and microwave dielectric properties of Li2Mg3TiO6-xwt%ZBS
and Li2Mg3TiO6-xwt%LBS were investigated, respectively. What's more,
Fig. 1. XRD patterns of Li2Mg3TiO6 ceramics doped with (a) xwt% ZBS glass
they were compared to help us find the best sintering additive.
and (b) xwt% LBS glass sintered at different temperatures.

2. Experimental procedure

Li2Mg3TiO6 ceramics were prepared through a conventional solid-

state reaction route. We used high-purity oxide powders of
Li2CO3(99%), MgO(98%) and TiO2(99.9%) as raw materials. Firstly,
they were mixed according to the formula of Li2Mg3TiO6 and milled
with ZrO2 balls as grinding media in deionized water for 8 h. After
being milled, the obtained slurries were dried off at 100 °C in the air.
Then, all mixtures were calcined at 1000 °C for 4 h with a heating rate
of 5 °C/min. The raw materials of ZnO, Li2CO3, B2O3 and SiO2 were
weighted according to the mole proportion of 6:3:1for ZBS glass and
50:40.24:9.76 for LBS glass, respectively. The burdened raw materials
were mixed adequately by high energy ball milling. After dried, the
mixtures were calcined at 1400 °C (ZBS) and 1050 °C (LBS) for 1 h. Then
quickly poured the molten glass into deionized water and cool it
thoroughly. The ZBS and LBS glasses were obtained [13,15].
Li2Mg3TiO6 was remilled with 0-8 wt% ZBS/LBS glass and ZrO2 balls in
deionized water for 8 h and dried. Afterwards, the granulated powders
were pressed into disks with 10 mm in diameter and about 5 mm in
height and then sintered at 975–1075 °C for 6 h in the air with the
heating rate of 4 °C/min.
The crystalline phases of Li2Mg3TiO6 ceramics with different con-
tents of ZBS and LBS glasses were investigated by X-ray diffraction
(Rigaku D/max 2550 PC, Tokyo, Japan) with Cu Ka radiation. The
microstructures of ceramics were observed by scanning electron mi-
Fig. 2. The SEM photographs of Li2Mg3TiO6 ceramics doped with (a) 0 wt%
croscopy (ZEISS MERLIN Compact, Germany) and the components of ZBS, 1350 °C, (b) 2 wt%ZBS, 1075 °C, (c) 4 wt%ZBS, 1025 °C, (d) 6 wt%ZBS,
sample were analyzed by an energy dispersive spectrometer (EDS). 1025 °C, (e)8 wt%ZBS, 1025 °C, (f) EDS spectrum and data of A, (g) 2 wt%LBS,
The microwave dielectric properties of all samples were measured 1075 °C, (h) 4 wt%LBS, 1050 °C, (i) 6 wt%ZBS, 1025 °C, (j) 8 wt%ZBS, 1025 °C.
by a network analyzer (N5234A, Agilent Co, America) with the fre-
quency range of 5–12 GHz [16,17]. The temperature coefficient of re-
lattice interstitial site and lead to the enlargement of unit cell volume.
sonant frequency (τƒ) was measured in the temperature range from
However, the peak position no longer shifts for x ≥ 6, indicating the
25 °C to 85 °C and was calculated by the following formula:
solid solubility limit of Si4+ in the lattice. As shown in Fig. 1(b), for LBS
f85 − f25 doped in Li2Mg3TiO6 ceramics, all XRD patterns exhibit Li2Mg3TiO6
τf = × 106 (ppm / °C )
f25 (85 − 25) (1) phase and the second phase Mg2SiO4, the same as Li2Mg3TiO6-xwt%
ZBS ceramics.
where f85 and f25 were the resonant frequencies at 85 °C and 25 °C, The SEM photographs of Li2Mg3TiO6 ceramics with different
respectively. amounts of ZBS and LBS glass are exhibited in Fig. 2. The average grain
size increases with the increase of ZBS/LBS content due to elevated
3. Results and discussions boundary and diffusion conefficient caused by liquid phase sintering
[8,19]. Fig. 2 (a)∼(e) demonstrate the microstructures of Li2Mg3TiO6-
Fig. 1 (a) and (b) display the XRD patterns of Li2Mg3TiO6 ceramics xwt%ZBS ceramics (0 ≤ x ≤ 8). It can be seen that the porosity of the
doped with xwt% ZBS and LBS glass (0 ≤ x ≤ 8) sintered at different Li2Mg3TiO6 ceramics decrease obviously with the amounts of ZBS glass
temperatures, respectively. From Fig. 1 (a), all samples exhibit the increasing from 2 wt% to 4 wt%, which indicates the addition of ZBS
Li2Mg3SnO6-like (JCPDS #39–0932) cubic phase with ordered rock salt glass accelerates a dense Li2Mg3TiO6 ceramic through liquid phase
structure and a little Mg2SiO4-like phase could be observed in all sintering. Dense microstructures are formed of Li2Mg3TiO6 ceramics
samples, which could be caused by the addition of ZBS glass. The main with 4 wt%ZBS. However, a large amount of liquid phase could be
peaks of Li2Mg3TiO6 angle are higher compared to Li2Mg3SnO6-like found in Li2Mg3TiO6 ceramics doped 6-8 wt% ZBS glass sintered at
because the ionic radius of Ti4+(R = 0.605 Å, CN = 6) is smaller than 1025 °C, which could have a negative effect on microwave dielectric
that of Sn4+(R = 0.69 Å, CN = 6) [18]. In addition, taking the crystal properties. Furthermore, Fig. 2(f) is the EDS spectrums of x = 4 sintered
plane (200) as a representative, it can be seen that the peak position at 1025 °C, which confirms that there is indeed silicon ion into the
slightly shifts to lower angles with the increase of ZBS content. This lattice. Fig. 2. (g)∼(j) show the microstructures of Li2Mg3TiO6-xwt%
result can be attributed that a small amount of Si4+ ions dissolve in the LBS ceramics (2 ≤ x ≤ 8), the pores are present on the surface of

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Fig. 3. The variations of (a) density (b) ɛr and (c) Q×f values of Li2Mg3TiO6- Fig. 4. The variations of (a) density (b) ɛr and (c) Q×f values of Li2Mg3TiO6-
xwt% ZBS (0 ≤ x ≤ 8) ceramics at different sintering temperatures. xwt% LBS (0 ≤ x ≤ 8) ceramics at different sintering temperatures.

Li2Mg3TiO6-2wt%LBS and the samples are not densified. Li2Mg3TiO6

ceramics doped with 4 wt% and 6 wt%LBS glass have fewer pores and
higher density. The ceramic surface has the distinct glass phase when
the LBS addition amount is 8 wt%, which affects the microwave prop-
erties significantly.
Fig. 3 shows the variations of densities and microwave dielectric
properties of Li2Mg3TiO6-xwt% ZBS (0 ≤ x ≤ 8) ceramics at different
sintering temperatures. In Fig. 3(a), the maximum bulk density of
3.37 g/cm3 is obtained at 1350 °C. The bulk densities of Li2Mg3TiO6
with 2 wt% ZBS glass increase continually when sintering temperatures
rise from 975 °C to 1075 °C, which indicates that the amount of the
produced liquid phase at x = 2 should be not enough to ensure the
liquid phase sintering mechanism for Li2Mg3TiO6 ceramics. Besides, the
bulk densities of Li2Mg3TiO6 ceramics doped with 4-8 wt% ZBS glass
increase when sintering temperatures rise from 975 °C to 1025 °C, then
fluctuate slightly. Besides, the largest bulk density is obtained by
adding 4 wt%ZBS glass sintered at 1025 °C, which illustrates that it is
enough to ensure the liquid phase sintering of the sample and the ex- Fig. 5. The Q×f values of Li2Mg3TiO6-4wt%ZBS and Li2Mg3TiO6-4wt%LBS
cessive liquid phase will hinder the sintering process, resulting in a ceramics sintered at different temperatures.
decrease in density. It is reported that the Q×f values of ceramics are
influenced by intrinsic factors and extrinsic factors. The intrinsic factors the ɛr and Q×f values with the Li2Mg3TiO6-xwt%ZBS ceramics. Besides,
are related to lattice vibration modes, while the extrinsic factors include similar to ZBS, the properties of LBS glass have an important influence
oxygen vacancies, grain boundaries, second phases and densification on microwave dielectric properties of Li2Mg3TiO6 ceramics.
[20,21]. In Fig. 3(b) and (c), the ɛr and Q×f values of Li2Mg3TiO6 Fig. 5 demonstrates the Q×f values of Li2Mg3TiO6-4wt%ZBS and
ceramics have the similar trend with bulk densities as the sintering Li2Mg3TiO6-4wt%LBS ceramics sintered at different temperatures. It
temperatures increase. The values of ɛr and Q×f increase first to the can be informed that Li2Mg3TiO6-4wt%ZBS has the highest Q×f value
maximum due to the improvement of the densification and then de- of 138,800 GHz sintered at 1025 °C, while the best value of Li2Mg3TiO6-
crease with the increase of sintering temperatures and ZBS content 4wt%LBS is 130,900 GHz sintered at 1050 °C for 6 h. That the Q×f
which is caused by the inhomogeneous grain morphology, incon- values of Li2Mg3TiO6-4wt%ZBS are higher can be attributed to the
spicuous grain boundary and excessive liquid phase. It can be observed dense and homogeneous morphology [22].
in Fig. 3(b) that the ɛr of Li2Mg3TiO6 ceramics doped with 6-8 wt% ZBS Fig. 6 shows the τƒ values of Li2Mg3TiO6-xwt%ZBS and Li2Mg3TiO6-
reduce monotonically because of the smaller dielectric constant of xwt%LBS ceramics as a function of x sintered at optimum temperatures.
Mg2SiO4 (ɛr = 6.8). Besides, the decrease of Q×f values when x > 4 In previous reports, the τƒ value was influenced by the second phase,
may be result in the reduction of densification and the formation of the octahedral distortion, bond valence and energy [23]. It is reported that
second phase. What's more, the higher dielectric loss of sintering ad- the τƒ values of the composite ceramics could be calculated by using
ditive ZBS is also a major factor affecting the Q×f values. Lichtenecker empirical logarithmic rule [24]:
Fig. 4(a) illustrates the densities of Li2Mg3TiO6-xwt% LBS
(0 ≤ x ≤ 8) ceramics sintered at different temperatures. As the sin- τf = v1 τ f1 + v2 τ f2 (2)
tering temperatures increase, the bulk densities of Li2Mg3TiO6-2wt%
LBS keep increasing, the densities of Li2Mg3TiO6-xwt% LBS (4 ≤ x ≤ 8) in our work, vi and τ fi are the volume fractions and the τƒ values of the
ceramics increase first and then decrease. When x = 4, the density pure Li2Mg3TiO6 and Mg2SiO4. We observe that the τƒ of Li2Mg3TiO6
reaches the maximum at 1050 °C, while that of x = 6 and 8 get the ceramics decrease slightly with the content of ZBS and LBS glass in-
largest at 1325 °C. Fig. 4(b) and (c) show the ɛr and Q×f values of creasing because of the small difference between the τƒ values of
Li2Mg3TiO6-xwt% LBS (0 ≤ x ≤ 8) ceramics at different sintering Li2Mg3TiO6ceramics (−39 ppm/°C) and Mg2SiO4 ceramics (-67 ppm/
temperatures. It can be observed that the ɛr and Q×f values have the °C).
similar trend with bulk densities. The formation of the second phase In general, the microwave properties of Li2Mg3TiO6 ceramics doped
Mg2SiO4 in Li2Mg3TiO6-xwt%LBS ceramics has the similar effects on with 4 wt%ZBS or 4 wt%LBS are great when sintered at lower tem-
peratures. Table 1 presents the sintering temperatures and microwave

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P. Zhang et al. Materials Chemistry and Physics 227 (2019) 130–133

Foundation of China (No. 61671323) and the Natural Science

Foundation of Hebei Province, China (No. E2017202011).

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This work was supported by the National Natural Science

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