J.Cent.SouthUniv.

(2012) 19: 20942100

DOI: 10.1007/s1177101212508

Comparativecharacteristicsofyttriumoxideand
yttriumnitricacid doping inZnOvaristorceramics
XUDong()1, 2, 3,TANGDongmei()1,4,JIAOLei()1,
YUANHongming()5,6, ZHAOGuoping()1, CHENGXiaonong()1,4
1.SchoolofMaterialsScienceandEngineering,JiangsuUniversity,Zhenjiang212013,China
2.KeyLaboratoryofSemiconductorMaterialsScience,InstituteofSemiconductors,
ChineseAcademyofSciences,Beijing100083,China
3.StateKeyLaboratoryofElectricalInsulationandPowerEquipment(XianJiaotongUniversity),
Xian710049,China
4.ChangzhouEngineeringResearchInstitute, JiangsuUniversity,Changzhou213000,China
5.StateKeyLaboratoryofInorganicSynthesisandPreparativeChemistry (JilinUniversity),
Changchun130012,China
6. CollegeofChemistry,JilinUniversity,Changchun130012,China
CentralSouthUniversityPressandSpringerVerlagBerlinHeidelberg2012
Abstract: The effect of different molar ratios of Y2O3 and Y(NO3)3 on the microstructure and electrical response of
ZnOBi2O3based varistor ceramicssintered at 1000 Cwasinvestigated,and the mechanismby whichthis doping improvesthe
electricalcharacteristicsofZnOBi2O3basedvaristorceramicswasdiscussed.WithincreasingamountsofY(NO3)3 orY2O3 inthe
starting composition, Y2O3, Sb2O4 and Ycontaining Birich phase form, and the average grain size significantly decreases. The
averagegrainsizesignificantly decreases as thecontentsofrareearthcompoundsofY(NO3)3 orY2O3 increase.Themaximumvalue
of the nonlinear coefficient is found at 0.16% Y(NO3)3 or 0.02% Y2O3 (molar fraction) doped varistor ceramics, and thereis an
increaseof122%or35%comparedwiththevaristorceramicswithoutY(NO3)3 orY2O3.ThethresholdvoltageVT ofY(NO3)3 and
Y2O3 reachesat1460V/mmand1035V/mm,respectively.TheresultsalsoshowthatvaristorsampledopedwithY(NO3)3 hasa
remarkablymorehomogeneousanddensermicrostructureincomparisontothesampledopedwithY2O3.
Keywords:ceramics varistorrareearthmicrostructureelectricalproperties

1Introduction
Commercialvaristorceramicsareusuallymadebya
solid state process using ZnO particles with dopant
oxides, such as Bi2O3, Sb2O3, Co2O3, MnO2 and Cr2O3.
Themixedpowderisthenpressedandsinteredatahigh
temperature [12]. This leads to a final microstructure,
which,inthe ideal situation, is constituted ofa uniform
grain size without porosity, segregated at grain
boundaries, and homogeneously distributed crystalline
secondary phases such asthe spinel type Zn7Sb2O12 and
pyrochlore type Zn2Bi3Sb3O14 [34]. The conducting
ZnOis surrounded by Bi2O3 phase, that isaresult from
the liquid phase at the sintering temperature.Therefore,

the kind, the concentration and the distribution of both

the dopant and the corresponding created phases on
sintering, determine the final microstructure and the
electrical properties of the obtained varistor material
[57].
Recently,ithasbeenconfirmedthatitispossibleto
improvetheelectricalcharacteristicsbytheintroduction
of Y2O3 to the varistor ceramics [811]. BERNIK et al
[12] reported that the microstructural and electrical
characteristics of ZnOBi2O3based varistor ceramics
doped with Y2O3 in the range from 0 to 0.9% (molar
fraction) were investigated. LIU et al [13] discussed
ZnOBi2O3based varistor ceramics doped with 03%
Y2O3. XU et al [14] reported Y2O3doped ZnOBi2O3
basedvaristorceramicssinteredat1100C.Theresults

Foundationitem:Project(BK2011243)supportedbytheNaturalScienceFoundationofJiangsuProvince,ChinaProject(EIPE11204)supportedbytheState
KeyLaboratoryofElectricalInsulationandPowerEquipment,ChinaProject(KF201104)supportedbytheStateKeyLaboratoryofNew
CeramicandFineProcessing,ChinaProject(KFJJ201105)supportedbytheOpeningProgramofStatekeyLaboratoryofElectronicThin
Films and Integrated Devices, China Project(201122) supported by the State Key Laboratory of Inorganic Synthesis and Preparative
Chemistry ofJilin University,ChinaProject(10KJD430002)supportedbythe Universities NaturalScienceResearchProjectofJiangsu
Province,ChinaProject(11JDG084)supportedbytheResearch FoundationofJiangsuUniversity,China
Receiveddate:20111025Accepteddate:20120210
Correspondingauthor:XUDong,PhDTel:+8651188797633Email:frank@ujs.edu.cn

J. Cent.SouthUniv. (2012) 19: 20942100

showedthatwiththeadditionof0.60%Y2O3,thevaristor
ceramics exhibited comparatively better comprehensive
electrical properties, such as the threshold voltage was
482 V/mm, the nonlinear coefficient was 34.8 and the
leakage current was 0.17 A. Y(NO3)36H2Odoped
varistor ceramics sintered at 1 100 C can be found in
our previous research [2]. The results showed that the
addition of 0.16% Y(NO3)36H2O to the ZnOBi2O3
basedvaristorceramicsproducedtheoptimumelectrical
properties,namelythethresholdvoltagewas425V/mm,
the nonlinear coefficient was 73.9 and the leakage
currentwas1.78A.Inthiswork,thevaristorceramics
werebothsinteredat1100C,butthehightemperature
sintering process had no advantage in both technology
andeconomy.
Inthiswork,theeffectofY2O3 andY(NO3)3 onthe
microstructure and electrical response of ZnOBi2O3
based varistor ceramics sintered at a lower sintering
temperature, such as 1 000 Cis studied, and the
mechanismby whichthisdopingimprovestheelectrical
characteristics of ZnOBi2O3based varistor ceramics is
discussed.

2095

silverpastewascoatedonbothfacesofthesamplesand
the silver electrodes formed by heating at 600 C for
10 min. The electrodes were 5 mm in diameter. The
voltagecurrent (VI) characteristics were measured
usingCJPCJ1001.Thenominalvaristorvoltages(VN)at
0.1and1.0mAweremeasured, andthethresholdvoltage
VT (VT=VN/ttisthethicknessofthesampleinmm)and
the nonlinear coefficient (=1/lg(V1 mA/V0.1 mA)) were
determined. The leakage current (IL) was measured at
0.75VN [56, 8, 1720]. The crystalline phases were
identified by an Xray diffractometry (XRD, Rigaku
D/max2200,Japan)usingaCuK radiation.Ascanning
electronmicroscope(SEM,FEIQUANTA400)wasused
toexaminethesurfacemicrostructure.

3Resultsanddiscussion

2Experimental

XRD patterns of the samples doped without and

with various amounts of Y(NO3)3 or Y2O3 sintered at
1 000 C for 2 h are shown in Fig. 1. It is well known
thatZnOBi2O3basedvaristorceramicstypicallyconsist
of ZnO grain, spinel and intergranular Birich phase. In
thesamplewithoutY(NO3)3 orY2O3,theZnOphase,the
Zn 7 Sb2 O12 typespinelphase,Bi 3 Zn2 Sb3 O14 andBi 2 O3

Y2O3 doped ZnOBi2O3based varistor samples

were gained with a composition of (96.5x)% ZnO,
0.7% Bi2O3, 1.0% Sb2O3, 0.8% Co2O3, 0.5% Cr2O3,
0.5%MnO2 andx%Y2O3,for x=0,0.02,0.08,0.20and
1.00(molarfraction,sampleslabeledasY0,Y1,Y2,Y3
and Y4, respectively). After milling, the mixture was
dried at 70 C for 24 h, and then the powder was
uniaxially pressed into discs of 12 mm in diameter and
2mminthickness.
Y(NO3)3 doped ZnOBi2O3based varistor samples
wereobtainedintheproportions of (96.5x)% ZnO,0.7%
Bi2O3, 1.0% Sb2O3, 0.8% Co2O3, 0.5% Cr2O3, 0.5%
MnO2 and x% Y(NO3)36H2O, for x=0, 0.04, 0.16, 0.40
and2.00(sampleslabeledasYD0,YD1,YD2,YD3and
YD4,respectively).Aftermilling,themixturewasdried
at 70C for 24 h, and then the powder was calcined at
700Cfor2hinair.Thecalcinedpowdermixturewent
through a second milling for 1 h to eliminate large
powderlumps.Thepowderswerethendriedandpressed
into discs of ~12 mm in diameter and 2.0 mm in
thickness.
The pressed discs were sintered in air at 1 000 C
(2 h dwell time), using a heating rate of 5 C/min and
then cooled in the furnace. The sintered samples were
lapped and polished and then the final samples were
about 10mmin diameter and 1.0 mm in thickness.The
bulk density of the samples was measured in terms of
theirmass andvolume [1516].
ForthecharacterizationofDCcurrentvoltage,the

Fig. 1 XRD patterns of ZnOBi2O3based varistor ceramics

dopedwithvariousamountsofY(NO3)3 orY2O3: (a)Y(NO3)3
(b)Y2O3

2096

phase are identified. However, in samples doped with

Y(NO3)3 or Y2O3,thepeakoftheZn7Sb2O12typespinel
phase becomes weaker with the addition of Y(NO3)3 or
Y2O3 [21],andnearlyvanisheswhentheamountof Y2O3
is increased to 1.00%, while that of the Y2O3 phase
increases at the same time, which agrees with the
previous research [13]. With increasing amounts of
Y(NO3)3 or Y2O3 in the starting composition, the
Ycontaining Birich phase (Bi1.9Y0.1O3 phase according
toJCPDF390275),theY2O3 phaseandtheSb2O4 phase
are revealed by the XRD analysis. The addition of
Y(NO3)3 or Y2O3 affects the time that the mixture is
spentintheliquidphase,andsince itbecomeslonger,the
vaporization of Bi2O3 from the ZnOBi2O3based
varistor ceramics becomes significant [5, 17]. In the
meantime, thedoping with Y(NO3)3 or Y2O3 affects the
formation and decomposition of the Bi3Zn2Sb3O14
pyrochlore, which promotes the generation of the new
phases,suchastheYcontainingBirichphase,theY2O3
phase and theSb2O4 phase.

J. Cent. South Univ. (2012) 19: 20942100

SEMmicrographsoftheZnOBi2O3basedvaristors
doped with various amounts of Y(NO3)3 or Y2O3
sinteringat 1000Cfor 2hare givenin Figs. 2 and 3,
respectively. The SEM micrographs indicate that the
average grain sizesignificantlydecreases as the content
of Y(NO3)3 or Y2O3 increases. At the same time, the
crystallite sizes of the Y2O3 phases become smaller but
the quantities increase dramatically, and there is little
different from the sample without Y(NO3)3 or Y2O3
doping. The majority of the new phases is much more
segregated at the multiple ZnO grain junctions than
between two ZnO grains. Since the diameter of the
rareearth cation islarger than that ofthe Zn2+ cation, it
is possible that the yttrium cation is not properly
dissolvedintheZnOgrains.WithincreasingY(NO3)3 or
Y2O3 content,theYrichphasebecomesmoredistributed
atthemultipleZnOgrainjunctionsandtheYrichphase
between two ZnO grains is more discontinuously
distributed [8, 2122]. At the same time, the size of
theZnOgrainsdecreasesuniformlywhentheamountof

Fig. 2 SEM images of ZnOBi2O3based

varistor ceramics doped with various
amounts of Y(NO3)3: (a) YD0 (b)YD1
(c)YD2(d)YD3(e)YD4

J. Cent.SouthUniv. (2012) 19: 20942100

2097

Fig.3SEM imagesofZnOBi2O3based
varistor ceramics doped with various
amountsofY2O3: (a)Y0(b)Y1(c)Y2
(d)Y3(e)Y4

Y(NO3)3 or Y2O3 increases, which would have some

influence on the electrical properties of varistor
ceramics.
The relative density D with various amounts of
Y(NO3)3 or Y2O3 doped ZnOBi2O3based varistor
ceramicssinteredat1000Cfor2hisshowninFig.4.
TheresultsrevealthatdopingwithY(NO3)3 orY2O3 has
a little influence on the relative density of ZnOBi2O3
basedvaristorceramics[2,14].WithincreasingY(NO3)3
orY2O3 content, therelativedensitychangesintherange
of 94.1%97.2%. With increasing the amount of
Y(NO3)3, the relative density of the Y(NO3)3 doped
ZnOBi2O3based varistor ceramics increases and then
decreases. Obviously, in all cases, the extremum of the
relativedensity is reachedwith0.08%Y2O3.
The threshold voltage VT with various amounts of
Y(NO3)3 or Y2O3 doped ZnOBi2O3based varistor
ceramicssinteredat1000Cfor2hisshowninFig.5.
When increasing the Y(NO3)3 content, the threshold
voltageismarkedlyincreasedintherangeof535

Fig. 4 Density of ZnOBi2O3based varistor ceramics doped

with variousamountsof Y(NO3)3 orY2O3

1460V/mmalongwithadecreaseinaveragegrainsize
of ZnO (Fig. 2). When increasing the Y2O3content, the
threshold voltage is markedly increased in the range

2098

Fig.5 ThresholdvoltageofZnOBi2O3basedvaristorceramics
dopedwith variousamountsof Y(NO3)3 orY2O3

of 5601 035 V/mm along with a decrease in average

grain size of ZnO (Fig. 3). At the same time, the
breakdown voltages per grain boundary of the samples
areallintherangeof23V,accordingtoRefs.[2324].
The breakdown voltage per grain boundary (Vgb) is
determinedfromtheexpressionVgb=V1 mA/n=dVT,where
n is the number of grain boundaries arranged as the
seriesbetweenbothelectrodesanddistheaveragegrain
size. The threshold voltage increases as the grain size
decreases. Thesmaller the grains size is, the higher the
thresholdvoltageis.
The nonlinearcoefficientwithvariousamountsof
Y(NO3)3 orY2O3 ofZnOBi2O3basedvaristorceramics
sintered at 1 000 C for 2 h is shown in Fig. 6. For
Y(NO3)3 or Y2O3 doped ZnOBi2O3based varistor
ceramics, the nonlinear coefficient initially increases
then decreases with the increase of Y(NO3)3 or Y2O3
content. The relationship between the nonlinear
coefficient and the amount of earth oxide additive
reveals an upsidedown Ushape curve, which is
unsymmetrical. The maximum value of the nonlinear
coefficientisobtainedin0.16%Y(NO3)3 or0.02%Y2O3
doped varistor ceramics, andithasan increase of 122%
or 35% when compared with the varistor ceramics
without Y(NO3)3 or Y2O3, respectively. The significant
improvementof the nonlinearcoefficientobtainedforthe
varistorceramicswithY(NO3)3 canbeaccountedforthe
microstructure uniformity and narrowed grain size
distribution.
The leakage current IL with various amounts of
Y(NO3)3 orY2O3 ofZnOBi2O3basedvaristorceramics
sintered at 1 000 C for 2 h is shown in Fig. 7. It is
especiallymeaningfulthattheleakagecurrentisdirectly
related to degradation and reliability because the
leakagecurrentshouldbeaslowaspossibleforvarious

J. Cent. South Univ. (2012) 19: 20942100

Fig. 6 Nonlinear coefficient of ZnOBi2O3based varistor

ceramics dopedwithvariousamountsof Y(NO3)3 orY2O3

Fig. 7Leakage current of ZnOBi2O3based varistor ceramics

dopedwith variousamountsof Y(NO3)3 orY2O3

applications [22]. For Y2O3 doped ZnOBi2O3based

varistor ceramics, when the amount of Y2O3 increases
from 0% to 1.0%, the leakage current is very low and
only shows little change. For Y(NO3)3 doped ZnO
Bi2O3based varistor ceramics, when the amount of
Y(NO3)3 is less than 0.40%, the leakage current shows
little change, but when the amount of Y(NO3)3 is more
than0.40%,theleakagecurrentincreasessharply,byup
to50A,andthevaristorceramicswouldnotbeapplied
ifthereisahighleakagecurrent.Atthesametime,when
the ZnOBi2O3based varistor ceramics are doped with
2.00% Y(NO3)3, there is an increase of amount the
secondphases,suchasZn7Sb2O12typespinelphaseand
Bi3Zn2Sb3O14type pyrochlore phase. When the amount
ofthesecondphasesiscomparedwiththeamountofthe
ZnOphases, theuniformity of the microstructure would
become nonuniform. Consequently, the nonlinear
coefficient decreases,and leakage current increases. In
general,thevariationoftheleakagecurrent isoppositeto
thatofthenonlinearcoefficient.Theleakagecurrentisa

J. Cent.SouthUniv. (2012) 19: 20942100

resultofmostoftheelectronspassingovertheSchottky
barrier at grain boundaries. Therefore, the lower the
barrierheightis,thehighertheleakagecurrentbecomes,
and the lower the nonlinear coefficient is [5, 19, 22,
2526]. It is believed that the decrease in the leakage
current can be attributed to an increase in activation
energy (the average energy needed for electrons to
overcome the Schottky barrier) and the homogeneous
distribution of the limited amount of varistor dopants
availableinthesesamples.
Figure 8 shows the electric fieldcurrent density
(EJ)curvesofZnOBi2O3basedvaristorceramicswith
various contents of Y(NO3)3 or Y2O3. The curves show
thattheconductioncharacteristicshavedividedintotwo
regions:alinearregionbeforethebreakdownfieldanda
nonlinearregionafterthebreakdownfield.Thesharper
the knee of the curves between the two regions is, the
betterthenonlinearpropertiesare[27].Itisknownthat
the sharper the knee of the curves between the linear
regionandthebreakdownfieldis,thebetterthenonlinear
characteristic is, in other words, the threshold voltage
VT,thenonlinearcoefficient,andtheleakagecurrentIL
aredeterminedbythe EJcurves.Ascanbeseenfrom

2099

Fig. 8(a), the EJ curves show that the nonlinear

propertiesincreaseintheorderofYD4YD0YD1
YD3YD2, and the threshold voltage increases in the
order of YD0YD1YD2YD3YD4. As can be
seen from Fig. 8(b), the EJ curves show that the
nonlinear properties increase in the order of Y0Y3
Y2Y4Y1,andthethresholdvoltageincreasesinthe
order of Y0Y1Y2Y3Y4. Narrower grain size
distribution indicates more uniform and more
homogeneous microstructure, which influences the
uniform conducting and increasing number of active
grain boundaries. The consequence is anincrease of the
nonlinearity coefficients and breakdown field. Varistor
sample doped with 0.16% Y(NO3)3 has a remarkably
more homogeneous and denser microstructure in
comparisontothesampledopedwith0.08% Y2O3.

4Conclusions
1)Theminutequantityofrareearthcompoundscan
remarkably develop the properties of ZnOBi2O3based
varistor ceramics. The average grain size significantly
decreases as the content of Y(NO3)3 or Y2O3 increases.
Atthesametime,thecrystallitesizesoftheY2O3 phases
become smaller butthe quantities increase dramatically,
and there is little difference from the sample without
Y(NO3)3 orY2O3 doping.
2)WiththeincreaseofthecontentofY(NO3)3 and
Y2O3, the threshold voltage is respectively increased in
the range of 5351 460 V/mm and 5601 035 V/mm
alongwithadecreaseinaveragegrainsizeofZnO.The
maximum value of thenonlinear coefficient is found at
0.16%Y(NO3)3 or0.02%Y2O3 dopedvaristorceramics,
and it has an increase of 122% or 35% compared with
thevaristorceramicswithoutY(NO3)3 orY2O3.
3)The leakage currentis very low and only shows
little change for Y2O3 doped ZnOBi2O3based varistor
ceramics. When the content of Y(NO3)3 is less than
0.40%, theleakagecurrent showslittlechange,butitwill
changeupto50Awhenthe contentof Y(NO3)3 ismore
than0.40%.
4) Varistor ceramic doped with Y(NO3)3 has a
remarkably more homogeneous and denser
microstructure in comparison to the sample doped with
Y2O3.

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Fig. 8 Electric fieldcurrent density (EJ) characteristics of

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