Journal of Alloys and Compounds 866 (2021) 158855

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Journal of Alloys and Compounds

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

Influence of La2O3 doping on the characteristics of ZnO linear resistors

Jianke Liu, Jiaojiao Chen, Ruiting Zhang, Jinfeng Su, Yinan Qiao, Xin Xie, Wenbin Cao
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Research Center for Semiconductor Materials and Devices, Shaanxi University of Science and Technology, Xi'an 710021, China

a r t i cl e i nfo a bstr ac t

Article history: ZnO linear resistors have anticipated application prospect in electrical and electronic industry, but the study
Received 2 November 2020 of La2O3 doping is still poor. In this paper, the ZnO linear resistors doped with Al2O3, MgO, SiO2 and La2O3
Received in revised form 11 January 2021 were prepared by the conventional solid-state sintering method, and the effects of La2O3 doping on the
Accepted 19 January 2021
microstructure and comprehensive electrical properties were studied. Structural and morphological char­
Available online 4 February 2021
acteristics of the samples were investigated by scanning electron microscope (SEM) and X-ray diffraction
(XRD) respectively. The property of resistivity-frequency reveals that the samples could be applied in high-
Keywords:
Nonlinear coefficient frequency electric field. The dielectric property indicates Maxwell-Wagner interfacial polarization exists in
Resistance temperature coefficient the matrixes. With La2O3 content of 1 wt%, ZnO linear resistors have the best linear performance: the grain
La2O3 doping size is relatively uniform, the resistance temperature coefficient αT is − 6.63 × 10−3/°C, and the nonlinear
ZnO linear resistors coefficient α is 1.09. The comprehensive analysis of the influence of La2O3 doping on the electrical properties
Resistance impedance characteristics is of important significance for preparing ZnO linear resistors with excellent electrical properties.
© 2021 Elsevier B.V. All rights reserved.

1. Introduction Sm2O3 addition can obviously improve the resistance temperature

ZnO is n-type semiconductor because of nonstoichiometric
composition with excess Zn (Zn1+xO) on interstitial sites. Over the
past few years, ZnO was widely used in the fields of semiconductor
resistance materials, solar energy materials, and fluorescent mate­
rials [1]. Owing to their advantages of big resistivity variation range,
large flow density, low nonlinear coefficient α, and small resistance
temperature coefficient αT. ZnO linear resistors have been ex­
tensively used in electrical appliances, transportation, communica­
tion, and household appliances and other fields [2,3].
In the late 1980s, researchers prepared ZnO linear resistors with
good linear volt-ampere (V-I) characteristics by adding some ad­
ditives such as Al2O3 and MgO, based on ZnO varistors [4–6]. By
adding Al2O3 and MgO, ZnAl2O4 and MgAl2O4 spinel phases form,
which effectively reduces the nonlinear coefficient. The earliest
studies on ZnO linear resistors are mainly about the influence of
matrix formulation and sintering system on the comprehensive
electrical properties [7,8]. In recent years, many researchers have
begun to pay attention to the addition of rare earth metal oxides,
such as Sm2O3, La2O3 and TiO2 in ZnO linear resistors [9–12]. Lisjak
et al. found that value of αT is positive with adding Sm2O3 to ZnO
linear resistors [9]. Zhu et al. found that appropriate amounts of
⁎
Corresponding author.
E-mail address: caowenbin@sust.edu.cn (W. Cao).
coefficient of ZnO linear resistors compared with the Sm2O3-free
samples, the resistance temperature coefficient is 0.19 × 10−4/°C and
the nonlinear coefficient is 1.2 without Sm2O3 [10]. The previous
work reported that ZnO linear resistors added with TiO2 could ex­
hibit excellent linearity [11]. Wang et al. introducing La2O3 as a do­
pant into the ZnO-MgO-NiO-Al2O3-SiO2 linear resistors found that
La2O3 doping can reduce the value of α, but the analyses of the effect
of La2O3 doping on the electrical properties are simple [12].
Based on the above considerations, for ZnO linear resistors, Al2O3
and MgO are the basic dopant and have important effect on the
electrical properties,La2O3 doping can reduce the nonlinearity
coefficient [12]. Meanwhile, the doping of TiO2 can also improve the
density of and grain uniformity [11]. In this work, the ZnO linear
resistors were prepared by the conventional solid-state sintering
procedure, and the effect of La2O3 doping on the microstructure was
studied in detail.
2. Experimental procedure
ZnO linear resistors with the mass compositions (83 - x) wt%
ZnO + 9 wt% Al2O3 + 5 wt% MgO + 2 wt% TiO2 + 1 wt% SiO2 + x wt%
La2O3 (x = 0, 0.5, 1, 1.5, or 2) was prepared by the conventional solid-
state sintering. First of all, the raw materials and deionized water
were mixed with ZrO2 balls using a planetary high-energy ball for
3 h, and then dried at 140 °C for 4 h. The powders were mixed with
2 wt% polyvinyl alcohol (PVA) binder. The final powders were

https://doi.org/10.1016/j.jallcom.2021.158855
0925-8388/© 2021 Elsevier B.V. All rights reserved.
J. Liu, J. Chen, R. Zhang et al.
obtained by drying and then pressed into green compacts with a
diameter of 8 mm and a thickness of 1.5 mm. The green bodies were
heated to 600 °C for 2 h, and then heated to 1340 °C for 3 h with a
speed of 5 °C/min, then cooled down to room temperature, so the
ZnO linear resistors were obtained. To determine the electrical
properties, the samples were painted with silver paste and heated to
600 °C for 10 min.
X-ray diffraction was used for crystalline phase analysis of the
samples (XRD, Model Rigaku-D/Max-2200PC, Japan) using Cu Kα
radiation. The XRD pattern was refined to determine the value of a
and c using Jade. The samples were polished and thermally etched,
and then microstructure was examined by scanning electron mi­
croscopy (SEM, S-4800, Japan). The grain sizes of more than 500
grains observed in different areas of the samples by SEM were
measured. Mean grain sizes of the ZnO linear resistors were statis­
tically determined based on the sizes and numbers of grains. The
current-voltage characteristic of the ZnO linear resistors were tested
with a Keithley 2410 high voltage source meter. Nonlinear coefficient
α was used to calculated based on the equation α = 1/lg(V1A/V0.01A),
where V1A and V0.01A represent the voltages of 1 A and 0.01 A, re­
spectively. The impedance-frequency performance of the samples
was measured by an inductance capacitance resistance (LCR) table
(Agilent 4980A, America). The resistance temperature coefficient αT
was determined by the equation αT= (R−R0)/(T − T0)/R0, where R and
R0 are the resistance values of ZnO linear resistors at temperature T
and T0 respectively.
3. Results and discussion
Fig. 1 shows the X-ray diffraction (XRD) patterns of the ZnO linear
resistors with different content of La2O3 (0 ≤ x ≤ 2 wt%). The results
reveal that, with the absence of La2O3 doping, ZnO phase, spinel
ZnAl2O4 phase, and a small amount of MgAl2O4 phase appear.
However, when the doping amount of La2O3 is 1 wt%, a new phase
appears. The XRD patterns show that the new phase is the La-rich,
the similar behavior was reported for La2O3-doped WO3 ceramics
[13], and the diffraction peak of La-rich phase gradually increases by
increasing La2O3 doping.
As is shown in Fig. 2, the changes of lattice parameters a and c
with the increase of La2O3 doping were further obtained using Jade,
indicating that the lattice parameters of the samples change slightly
with increasing La2O3 doping. The ionic radius of La3+ and Zn2+ differ
significantly, which are 1.06 Å and 0.74 Å respectively, making it
difficult for La3+ enter the ZnO lattice and replace Zn2+. La element
mainly exists at ZnO grain boundary in the form of La-rich phase.
The microstructure of the samples was revealed in detail by SEM
analysis. Fig. 3 shows the SEM images of samples doped with
Fig. 1. XRD patterns of the ZnO linear resistors under different doping contents of
La2O3.
2
Journal of Alloys and Compounds 866 (2021) 158855
Fig. 2. Variation curves of lattice parameters of the ZnO linear resistors with different
contents of La2O3.
different contents of La2O3. The samples are relatively dense with
different La2O3 content. However, when the doping content of La2O3
is greater than 1 wt%, the spinel phase and La-rich phase in the
samples produce obvious aggregation at the grain boundary, making
the ZnO grain vary greatly and distribute unevenly. The grain contact
is so close that the grain boundary does not appear to be connected
into a piece.
Fig. 4 and Fig. S1 show the EDX mappings of the ZnO linear re­
sistor with La2O3 doping of 1 wt%. As shown in Fig. 4b the EDX
mapping is composed of the areas with different colors, among
which, the red and yellow areas are obvious which correspond to Zn
and Al. The distribution of Mg is similar to that of Al, while O is
approximately evenly distributed in the whole sample (shown in Fig.
S1). Combining with XRD pattern analysis (Fig. 1), it can be seen that
the red areas in Fig. 4b correspond to ZnO phase, and yellow areas
correspond to ZnAl2O4 and MgAl2O4. Shown in Fig. S1, La is mainly
concentrated as the secondary phase and the others La uniformly
distribute in the others areas. Ti has similar distribution with La.
Combining with XRD patterns, it is noted that the areas enriched
with La and Ti correspond to the La-rich phase which contains Ti.
Therefore, shown in Fig. 4a, the lighter and larger grains are ZnO
grains, while the darker and smaller grains are mainly ZnAl2O4 and
MgAl2O4, with a small amount of La-rich phase.
Fig. 5 shows the change curve of the mean grain size obtained
according to the SEM image and the EDX mapping with increasing of
La2O3 doping. It shows that the mean grain size increases with in­
creasing La2O3 doping.
With increasing La2O3 doping from 0 to 1 wt%, the mean grain
size of ZnO grains changes slightly, but the mean grain size increases
with further increasing La2O3 doping from 1 to 2 wt%. According to
the above analysis from Fig. 4 and S1, a part of La exist in from of La-
rich phase at the grain boundary of ZnO, from XRD pattern, it is
noted that the region enriched with La corresponds to the La-rich
phase, the small amount uniformly distributed in other regions,
grain boundary migration become active and grain grows up with
increasing La2O3 doping, and the others La distributes uniformly in
the others areas. Grain growth occurs mainly due to grain boundary
migration, which is determined by the secondary phase distributing
at the grain boundary and defect existing in the others areas. The
secondary phases existing in the ZnO linear resistors are mainly
ZnAl2O4 and MgAl2O4, and small amounts of La-rich phase. So the
existence of La-rich phase may have slightly influence on the grain
boundary migration. But La distributing uniformly in the ZnO grains
and grain boundaries will affect the defect distribution, which fur­
ther affects the grain boundary migration and grain growth. So the
J. Liu, J. Chen, R. Zhang et al. Journal of Alloys and Compounds 866 (2021) 158855

Fig. 3. SEM images of the ZnO linear resistors with different contents of La2O3.

grain growth of ZnO grains is negligible with La doping less than

1 wt%, and obvious with La doping in the range from 1 to 2 wt%.
Fig. 6 shows the resistivity-frequency characteristic of the ZnO
linear resistors with different La2O3 doping. The resistivity of the
samples are steady-state for the frequency in the range from 10 kHz
to 2 MHz. However, under the electric field frequency of 10 kHz, the
resistivity decreases gradually with increasing test frequency, which
shows apparent frequency dispersion at different levels. Liu et al.
also studied the resistivity-frequency characteristic of ZnO linear
resistors with different MgO doping [14]. They found that the re­
sistivity remain unchanged for the frequency less than 0.1 MHz but
decrease with increasing frequency in the range from 0.1 to 2 MHz. It
reveals that the ZnO linear resistors obtained may be applied in
high-frequency electric field.
Meanwhile, the impedance-frequency characteristics with dif­
Fig. 5. Variation curves of the mean grain sizes of the ZnO linear resistors with dif­
ferent La2O3 doping were investigated, and the Nyquist plots were
ferent contents of La2O3.
obtained based on the equivalent circuit composed of parallel RC
elements in the range from 100 Hz to 2 MHz (shown in Fig. 7). The
Nyquist plots fitted by Z-View software with different La2O3 doping
Rgb
are all arcs, and the impedance of samples could be determined by: [Z (Rg + Rgb)]2 + Z" =
2 (3)
Rgb
Z = Rg + where Rg denotes the resistance of grain, Rgb denotes the resistance
1 + ( Rgb Cgb)2 (1)
of grain boundary, Cgb is the capacitance of grain boundary, and f is
electric field frequency, ω denotes circular frequency. From Eqs. (1)
Cgb Rgb2 to (3), they reveal that the circular arc in high-frequency regions
Z =
1 + ( Rgb Cgb)2 (2) corresponding to the resistivity of ZnO grain (ρg), and the circular arc
in low-frequency regions corresponding to the grain boundary (ρgb)

Fig. 4. SEM image (a) and corresponding EDX mapping (b) of ZnO linear resistor with La2O3 doping of 1 wt%. (For interpretation of the references to colour in this figure, the reader
is referred to the web version of this article.)

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J. Liu, J. Chen, R. Zhang et al. Journal of Alloys and Compounds 866 (2021) 158855

(in the range from 1 to 2 wt%), which is due to the uniform dis­
tribution of La2O3 in the ZnO grains and grain boundaries corre­
sponding with the effect of La2O3 doping on the grain size of ZnO.
ZnO is n-type semiconductor, showing negative temperature coef­
ficient (NTC) characteristics, and the ZnO linear resistors obtained
also show NTC characteristic with different contents of La2O3
doping.
It is known that ZnO linear resistors follow thermally activated
conductive mechanism. The resistivity and temperature of the
samples measured in the direct current 5 V electrical experiment
satisfy the following equation:

= ( E /kT)
0e (4)

E = 0 (5)
Fig. 6. The resistivity frequency characteristics curves of the ZnO linear resistors with
different contents of La2O3. where ρ is the resistivity of the samples, ρ0 is the resistivity of the
samples as the temperature approaches infinity, ∆Eσ is activation
energy, φ0 is the height of barrier at the grain boundary, k is the
Boltzmann’s constant, and T is the absolute temperature.
By further deformation
0
ln = ln 0 +
kT (6)

According to Eq. (6), the relationships of lnρ~1000/T for ZnO

Fig. 7. Nyquist plots of the ZnO linear resistors with different contents of La2O3.
[15]. Therefore, according to the intercept of the semicircle on the
actual axis, ρg and ρgb could be calculated listed in Table 1.
As shown in Table 1, the resistivity of grain boundaries (ρgb) are
much higher than that of grains (ρg), which accords with the prin­
ciple of "permeation conduction". Moreover, with increasing La2O3
doping, the value of ρg and ρgb increase. According to the analyses of
XRD patterns (Fig. 1) and EDX mappings (Fig. 4 and S1), a part of La3+
will enter ZnO lattice with La2O3 doping. So the vacancy compen­
sation of trivalent metal cation will occur, which increases the grain
resistivity [16]. Meanwhile, La-rich phase distributing in the grain
boundary hinders the conductive path between ZnO grains, leading
to increasing ρgb with increasing La2O3 doping. In addition, the
variation amplitude of ρgb is more extensive than that of ρg, in­
dicating that ρgb plays a dominant role in the electrical properties of
the samples.
Resistance temperature (R-T) characteristic is an important
property of the ZnO linear resistors, which is listed in Table 1. When
the content of La2O3 doping is low (0–1 wt%), the temperature
coefficient αT changes gently, with the La2O3 doping increasing to
1–2 wt%, the value of αT decreases by 33%. So the R-T characteristic of
the linear resistors is affected obviously with high content of La2O3
linear resistors with different La2O3 doping were obtained (shown in
Fig. 8), φ0 is obtained according to the slope of the fitting straight
line. The correlation factors R2 of the fitting are all greater than 0.97
in Fig. 8, indicating that the fitting line has a high relevant degree.
The conduction mechanism of the samples is the thermally activated
progress [17], which follows the Arrhenius type law. The calculation
results show that, with increasing La2O3 contents, the value of φ0
change in the range of 0.07868–0.15791 eV and the nonlinear coef­
ficients (α) are close to 1. When the doping amount of La2O3 is 1 wt%,
the minimum values of φ0 and α is 0.07868 eV and 1.09, respectively.
Similarly, Wang et al. studied the effect of La2O3 doping on the
electrical properties of ZnO-MgO-NiO-Al2O3-SiO2 linear resistors,
and found that addition of 0–1 mol% La2O3 results in a slight de­
crease of the nonlinear coefficient. The minimum value of nonlinear
coefficient is 1.16 [13]. With La2O3 doping, the ZnO linear resistors
obtained in this work have better linear current-voltage character­
istic compared with Wang et al.’s result. φ0 could be estimated by
the following equation:
e2Ns2
=
2Nd 0 (7)
where Ns and Nd denote the interfacial state concentration and
donor concentration respectively, ε denotes relative dielectric con­
stant. With the increase of La2O3 doping, the concentration of donor
impurity in samples also increases, thus reducing the barrier height
and improving the linear performance. However, the obvious dif­
ference in ionic radius between La3+ and Zn2+ leads to less solid
solution La formed in ZnO grains. Moreover, when the La2O3 content
is too high, the content of La2O3 phase increases at the grain
boundary, leading to the increase of the nonlinear coefficient.
The dielectric properties as a function of the frequency of the
samples are measured from 100 Hz to 2 MHz, as shown in Fig. 9. ZnO

Table 1
The electrical properties of the ZnO linear resistors with different contents of La2O3.

La2O3 ρg (Ω·cm) ρgb (kΩ·cm) φ0 (eV) α αT (×10-3) f (kHz) τ (×10-5)

0 wt% 48.01 23.11 0.09376 1.14 -6.96 7.70 2.07

0.5 wt% 60.41 23.06 0.10833 1.17 -6.89 4.52 3.52
1.0 wt% 97.43 65.48 0.07868 1.09 -6.63 1.61 9.87
1.5 wt% 99.35 139.41 0.15791 1.22 -8.14 0.50 31.75
2.0 wt% 142.78 355.73 0.08728 1.12 -8.23 6.08 2.62

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J. Liu, J. Chen, R. Zhang et al. Journal of Alloys and Compounds 866 (2021) 158855

Fig. 8. Arrehenius plots of numerically fitted ZnO linear resistors dc resistivity.

shows that the R-C network (a parallel circuit of capacitance and

resistance) can be used to analyze equivalently the electrical prop­
erties of the grain boundary in the samples. According to the char­
acteristics of the R-C circuit, the characteristic relaxation frequency f
and relaxation time τ of the fitting circuit is influenced by its grain
boundary resistance and capacitance. The specific expression is [20].

1
f=
2 Rgb Cgb (8)

= Rgb Cgb (9)

When the test frequency is less than the relaxation frequency, the
dielectric constant (ε) varies greatly with the frequency. When the
test frequency is larger than the relaxation frequency, ε decreases
Fig. 9. Frequency dependence of the dielectric properties of the ZnO linear resistors with frequency. When the doping amount of La2O3 is 1.5 wt%, the
with different contents of La2O3. relaxation time is the longest and the relaxation frequency is the
smallest, so its dielectric constant fluctuates minimally with the
frequency.
Fig. 10 shows the variation curve of dielectric loss (tanδ) with test
is a polar semiconductor, many polarization mechanisms may exist
frequency. It can be seen that tanδ decreases with the test frequency
in the ZnO linear resistors such as electrons, ions, and interfacial
polarization. He et al. found that interfacial polarization is the main
polarization mechanism for functional ceramics [18]. According to
the Maxwell- Wagner interfacial polarization model, due to uneven
distribution of internal phase, the defects such as grain boundary,
lattice distortion, impurity introduction will hinder the motion of
carriers, causing the accumulation at the grain boundary, resulting in
space charge polarization [19]. But the space charge polarization
cannot be established in a short time, there will be high permittivity
in lower frequency. With the increasing frequency of the applied
electric field, the partial polarization mechanism (such as space
charge polarization) cannot follow the alternating field, resulting in
relaxation the permittivity drops, as shown in Fig. 9. Liu et al. found
that permittivity constant of MgO doped ZnO linear resistors showed
a similar trend, indicating a similar microstructure [14].
With the increase of test frequency, the dielectric constant of
samples decreases gradually. The complex impedance analysis Fig. 10. The variation curve of dielectric loss (tanδ) with test frequency.

5
J. Liu, J. Chen, R. Zhang et al.
increases. When the test frequency is equal to 10 kHz, tanδ with
different content of La2O3 tends to be similar. Moreover, if the value
is small, the variation is slight with the frequency.
The phase composition and distribution of composite ceramic
resistors are complex, and the specific expression of dielectric loss
(tanδ) is shown in equation [21]:
tan = DP + DG (10)
where Dp represents the polarization loss, DG represents the leakage
loss. When ωτ"1, tanδ ≈ σ/ωε0εs, with the change of La2O3content, the
tanδ has the contrary tend with impedance-frequency character­
istics. When the test frequency is less than relaxation frequency, tanδ
decreases gradually with the frequency. When the test frequency is
larger than the relaxation frequency, tanδ varies little with the fre­
quency of the external electric field is stable.
4. Conclusions
1) With increasing La2O3 doping, ZnO linear resistors formed La-rich
phase based on ZnO, ZnAl2O4 and MgAl2O4 phases.
2) La3+ can be used as donor doping, to reduce the height barrier at
the grain boundary, further improving linear properties of ZnO
linear resistors.
3) ZnO linear resistors follow the Maxwell interface polarization
theory in an alternating electric field, taking space charge po­
larization as the main polarization mechanism. When the fre­
quency of the external circuit is less than the characteristic
relaxation frequency, the dielectric constant of resistance de­
creases significantly with increasing frequency, and the dielectric
loss (tanδ) is negatively correlated with the test frequency. When
the frequency of external circuit is greater than the characteristic
relaxation frequency, the dielectric constant of ZnO linear re­
sistors varies slightly with frequency, revealing that the constant
is more stable and the tanδ is smaller.
4) In ZnO linear resistors, the grain size is relatively uniform. When
the doping amount of La2O3 is 1 wt%, the resistance temperature
coefficient (αT) is − 6.63 × 10−3/°C, the minimum values of the
barrier height (φ0) and the nonlinear coefficient (α) are 0.0787 eV
and 1.09, respectively.
CRediT authorship contribution statement
All the authors have made great efforts in this paper. Jianke Liu,
Wenbin Cao, Jiaojiao Chen in terms of article writing and modify and
test have done a lot of work. Ruiting Zhang did a great many ex­
periments and prepared ZnO linear resistors with excellent electrical
properties. Jinfeng Su, Yinan Qiao and Xin Xie provided great help
in test.
Declaration of Competing Interest
The authors declare that they have no known competing fi­
nancial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Journal of Alloys and Compounds 866 (2021) 158855
Acknowledgements
We acknowledge the funding support from the National Natural
Science Foundation of China (51802183).
Appendix A. Supporting information
Supplementary data associated with this article can be found in
the online version at doi:10.1016/j.jallcom.2021.158855.
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