JOURNAL OF RARE EARTHS, Vol. 29, No. 11, Nov. 2011, P.

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Magnetic properties of rare earth HoCrO3 chromites

SU Yuling (㢣⥝⦆)1, ZHANG Jincang (ᓴ䞥ҧ)2, FENG Zhenjie (‫ރ‬ᤃᵄ)2, LI Zijiong (ᴢᄤ⚃)1, SHEN Yan (≜ች)1,
CAO Shixun (᳍Ϫ࢟)2
(1. Department of Physics, Zhengzhou University of Light Industry, Zhengzhou 450002, China; 2. Department of Physics, Shanghai University, Shanghai 200444, China)

Received 26 May 2011; revised 19 August 2011

Abstract: The temperature dependence of the magnetic properties was systemically studied by dc/ac magnetization and specific heat meas-
urement for heavy rare earth HoCrO3 chromites. The results revealed the existence of complex phase coexistence and competitive magnetic
behavior in HoCrO3 chromites. It was found that, in the region of higher temperature above 141.0 K, HoCrO3 behaved as a typical Cu-
rie-Weiss paramagnetic (PM). And in the region of low temperature, a novel magnetization behavior was observed with negative magnetiza-
tion (diamagnetism-like) characteristics under an external field of 100 Oe and M-T curves exhibited two symmetrical branches for field cool-
ing (FC) and zero field cooling (ZFC) modes. This behavior indicated the coexistence of canted antiferromagnetic (CAFM) and weak ferro-
magnetic (FM) phase. These also exhibited the existence of competition mechanism below characteristic temperature TN1=141.0 K and the
magnetic order of Ho ion below 7.5 K. The current complex magnetization might be attributed to the interaction between paramagnetic Ho3+
moments and canted Cr3+ moments.

Keywords: rare earth chromites; phase coexistence; magnetic interaction

The like-perovskite compounds with ABO3 structure ex- zation and susceptibility data under the assumption that the
hibit rich and varying physical properties, including mag- Ho ions interact with the Cr ions only and that the canting
netic, semiconducting, ferroelectric, multiferroic properties angle of the Cr moments against their antiferromagnetic axis
and so on. Thus it is interesting and meaningful in both the- is given by the Cr-Cr interaction alone. According to
ory and experiments[1–5]. Here, A is a large nonmagnetic al- Courths et al. and Kojima et al.[21,22], the Ho-Cr interaction is
kali, alkaline earth or rare-earth ion and B is a small transi- predominantly antisymmetric exchange. The Ho-Ho cou-
tion metal cation. Recently, rare-earth orthochromites pling has a dipolar and an exchange contribution of about the
LnCrO3 (Ln stands for rare-earth and yttrium) have aroused same magnitude. In this paper, we presented the results of
wide attention from many researchers due to their novel dc/ac magnetization measurements for polycrystalline Ho-
magnetic properties in the broad sense[6–8]. As a typical CrO3 chromites. From the magnetic properties and its de-
like-perovskite compounds, LnCrO3 exhibits various types pendence on temperature under FC and ZFC modes, a com-
of field induced spin reorientation wherein the weak ferro- plex phase coexistence with CAFM and weak FM phase was
magnetic moment becomes parallel to the direction of the found in heavy rare earth HoCrO3 chromites. These also
applied magnetic field[9–12]. In the cases H//a and c, the spin proved the existence of competition mechanism below char-
reorientations of (Ƚ1, Ƚ4)ĺȽ2 and (Ƚ1, Ƚ2)ĺȽ4 have been acteristic temperature TN1=141.0 K and the magnetic order
reported for various single crystal LnCrO3[13,14]. From a prin- of Ho ion below 7.5 K. These phenomena would be helpful
cipal point of view one has to make the distinction between to understand physical mechanism and possible application
Ln ions with an odd electrons, where the ground state always for heavy rare earth HoCrO3 chromites.
has a magnetic moment, and Ln ions with an even number of
electrons where the ground state may be (and often is) a
1 Experimental
singlet, which only shows induced magnetism; these systems
are conceptually different[15–17]. As one of such compounds, The experimental samples were prepared by the conven-
single crystal HoCrO3, with an even electron system, has tional solid-state reaction method with chemical formula
been studied by different methods[18–21], and they all show HoCrO3. Stoichiometric quantities of Ho2O3 (99.99%) and
that the chromium ions order at TN=140 K in a Ƚ2(Fx)[21] Cr2O3 (99.9%) were mixed, ground thoroughly in ethanol
configuration[19]. Hornreich et al.[18] analyzed their magneti- and calcined once for 24 h at 900 ºC. With intermediate

Foundation item: Project supported by the National Natural Science Foundation of China (10774097, 10875107), the Science & Technology Committee of Shang-
hai Municipality (08dj1400202), and the Natural Science Foundation of Henan Province (092300410138, 102300410108), the Doctoral Innova-
tion Fund of Zhengzhou University of Light Industry (2010BSJJ027)
Corresponding author: SU Yuling (E-mail: [email protected]; Tel.: +86-371-63556150)
DOI: 10.1016/S1002-0721(10)60598-4
SU Yuling et al., Magnetic properties of rare earth HoCrO3 chromites 1061

grinding, the products were pressed into pellets and sintered the region of low temperature. As the applied magnetic
at 1300 ºC for 24 h. Then the obtained pellets were thirdly fields increase, the “diamagnetism-like” behavior weakens,
reground, pressed into pellets and sintered again in air at e.g., H=1000 Oe, the negative magnetization disappears, and
1450 ºC for 50 h. And the final annealing was done in oxy- MZFC(T)>0 (the inset (b)). In order to see clearly the details
gen at 800 ºC for 5 h. X-ray diffraction patterns of samples of the changing characteristics, the differential coefficient
were obtained on XRD diffractometer (18 kW D/max-2500, |dM(ZF)/dT| is plotted by absolute value in Fig. 2 (the black
Cu-KĮ radiation), indicating that the samples are in good line as shown). The insets show the extended patterns by the
single phase of orthorhombic structure with the space group logical (the inset (a)) in the range of whole temperature. It
Pbnm (see Fig. 1). The lattice parameters obtained (a=0.523 can be seen that there exist two typical temperatures of
nm, b=0.551 nm and c=0.753 nm) is in good agreement with magnetic transition marked as TN1 and TN2 near 141.0 and
the previously results reported on lattice parameters[20]. 7.5 K, respectively. From FC curve in inset (a) and (b), the
Magnetic measurements were performed on the Physical MFC(T) shows a typical sharp transition from paramagnetism
Property Measurement System (PPMS-9, Q/D Inc., USA) (PM) at high temperature to ferromagnetism (FM) below
with the precision of 0.01 K for temperature and 0.2 Oe for 141.0 K. And this can only be seen from the logical zoom in
the magnetic field. All the M-H curves were recorded after the inset (a), which shows only weak FM in heavy rare earth
the sample was cooled down under ZFC conditions from HoCrO3 chromites. In addition, for ZFC curve, near TN1, a
paramagnetic state at room temperature. Heat capacity snake peak appears firstly and then the magnetization
measurements were realized on HoCrO3 by a relaxation changes suddenly to negative value with diamagnetism-like
method with a Quantum Design PPMS system and using a (DM) characteristics. According to earlier studies by Horn-
two IJ model analysis. A piece (18.6 mg) of the sample was reich et al., Bertaut et al. and Courths et al., T<TN1=141.0 K,
glued on the sample holder using Apiezon N grease, and the rare earth HoCrO3 chromites is possibly canted anti-
data were taken in the range of 2–300 K. ferromagnetic with a weak ferromagnetism[18,19,23].
The structural characteristic of heavy rare earth HoCrO3
chromites is shown in Fig. 3. Here, Fig. 3 is drawn from the
2 Results and discussion
results of XRD spectrum in Fig. 1 and Ref. [19]. For LnCrO3
The temperature dependence of ZFC and FC magnetiza- system, they crystallize in the orthorhombic structure at
tions MZFC(T) (empty circles) and MFC(T) (solid circles) room temperature (space group Pbnm) with four molecules
measured with an applied magnetic field of H=100 Oe for per unit cell, and exhibit so-called canted-antiferromagnetic
the experimental samples HoCrO3 is shown in Fig. 2. These (CAFM) order of localized Cr3+ moments (3d3, ȝeff=3.87 ȝB
M-T curves reveal an interesting and complex magnetic be- for a spin-only value) with Néel temperatures (TN1) of
havior. MFC(T) and MZFC(T) behave almost symmetrically 112–282 K[6–12] and a dielectric transition in the 472–516 K
change and only appear at the low temperature. And the (TE) range[13–15]. At the second Néel temperature TN2, the Ln
MFC(T) is positive in the whole region of temperature from 2 spins begin to reorder antiferromagnetically. The allowed
to 300 K, decreasing monotonously with increasing tem- spin configurations for the Cr3+ and Ln3+ sites at TN1<T<TN2
perature. In opposition, the MZFC(T) keeps negative values at are denoted as Ƚ1(AxGyCz;Cz), Ƚ2(FxCyGz;FxCy), and
low temperature and its absolute value |MZFC(T)| decreases Ƚ4(GxAyFz;Fz) in the Bertaut notation[16]. In CrO6 octahedrons
on warming. Usually, MZFC(T) always shows a positive value
and MFC(T) has the direction parallel to the applied field and
lies above MZFC(T) (both MZFC(T) and MFC(T) have the direc-
tion parallel to the applied field). It is said, for ZFC, that
there appears a novel “diamagnetism-like” behavior in

Fig. 2 Thermal magnetization curves at an applied field of 100 Oe

under ZFC and FC modes for experimental HoCrO3 sample
(The differential coefficient |dM(ZF)/dT| is also plotted and
the vertical arrows point several characteristic temperature.
Insets give the extended patterns by the logical (a) and the
Fig. 1 XRD spectrum for heavy rare earth HoCrO3 chromites at M-T curve at H=1000 Oe (b))
room temperature
1062 JOURNAL OF RARE EARTHS, Vol. 29, No. 11, Nov. 2011

pends on the competition between magneto-crystalline ani-

sotropy energy and the strength of applied field[23]. At low
measuring fields, not all the spins will be oriented in the di-
rection along the applied magnetic field. Then the significant
difference probably originates from an anti-parallel orienta-
tion of the Cr weak ferromagnetic moment and of the Ho
moment by Ho-Cr exchange interaction between FC and
ZFC. As the external applied fields enhances, more spins
will be oriented along the external magnetic field, and the
negative magnetization disappears.
In order to understand the magnetic properties in the
whole for the compound HoCrO3, we plot the reciprocal of
magnetic susceptibility Ȥí1 versus T curves in Fig. 4. In the
range of high temperature, Ȥí1 behaves linearly, indicating a
typical Curie-Weiss behavior fitted. This suggests that a
Fig. 3 Structural pattern for like-perovskite HoCrO3 compound paramagnetic region occurs above TN1. The data are ¿tted by the
Curie-Weiss (C-W) law as shown by dashed line in Fig. 4.
for perovskite cell, energy of 3d orbits splits into two state, From this, we calculate that the effective magnetic moment
one is composed of three kinds of 3d orbits with lower en- ȝeff and asymptotic paramagnetic Curie temperature TCW are
ergy called t2g, and the other is composed of two kinds with 11.55 ȝB and –24.0 K about for heavy rare earth HoCrO3
higher energy, called eg[24]. According to Hund’s rule, the chromites. The former is well in agreement with the theo-
three 3d electrons in Cr3+ occupy t2g state with parallel spin retical ones (11.28 ȝB) estimated from the contribution of a
and generate large spin on Cr3+ ion. If temperature is low spin-only Cr3+ and a free-ion Ho3+ moment. And later, the
enough, the superexchange (SE) interaction between the asymptotic Curie temperature TCW is negative, which sug-
large spins on the nearest Cr ions sandwiching O2í ion is gests the predominance of antiferromagnetic interactions in
generated, resulting in antiparallel spin configuration. Due to HoCrO3 chromites. The inset of Fig. 4 shows an extending
the orthorhombic distortion of HoCrO3 structure, Cr–O–Cr zoom in the region of low temperature below 141.0 K. It is
bond angle slightly deviates from 180º, resulting in residual obviously a non C-W behavior.
electronic spin originating from imperfect superexchange It is also very important to check the process characteris-
interaction and showing that the sample HoCrO3 is a canted tics of magnetic transition at temperature TN1 and TN2. For
antiferromagnet (CAFM) below TN1=141.0 K. The weak these, the temperature dependence of ac susceptibility was
ferromagnetic component is due to the AFM exchange in- measured at the different frequencies of 199.0, 987.0 and
teraction between Cr3+ spins[24,25]. And the allowed magnetic 3987.0 Hz (Fig. 5). It can be obviously seen that ac suscepti-
configuration is Ƚ2(FxCyGz;-Fx-Cy)[26] in the lower tempera- bility Mʾ presents a sharp peaks near TN1=141.0 K and a
ture region. As for the ZFC mode, it can be qualitatively ex- higher peak near TN2=7.5 K, respectively. It is well known
plained by assuming that during the ZFC magnetization that the frequency dependency of peak temperature may be
measurement (warming circle) Cr and Ho substructures are used to distinguish the magnetic characteristics such as spin
uncoupled and experience the same external applied fields.
Therefore, both substructures contribute independently to the
total magnetization. While, in the FC circle, the Cr substruc-
ture moments appear at TN1 and impose a local field over the
Ho3+ moments. That means the Ho substructure experiences
an internal field of the Cr substructure and the external field
due to the cooling in the presence of field. Therefore, the
MFC(T) is a superposition of the magnetizations of the Cr and
the Ho substructures, decreasing with the temperature in-
creasing. For the change at TN2=7.5 K, it would be caused
from rare earth Ho3+ spin ordering in antiferromagnetic ar-
rangement[19,27]. This spin ordering temperature is a little
higher than the one (TN2=6.5 K) in HoFeO3 with the known Fig. 4 Curie-Weiss approach by the dependence of the reciprocal of
magnetic structures of HoCrO3[23]. From the mechanism of dc magnetic susceptibility Ȥí1 on the temperature (An excel-
coexistence and competition, novel negative magnetization lent Curie-Weiss behavior can be seen in the region of high
(or diamagnetism-like) is resulted from the presence of dif- temperature above 141.0 K and the parameters, ȝeff and TCW
ferent magnetic entities (Ho3+, Cr3+) with AFM and FM in- can be well given. The inset shows an extending zoom in the
teractions. The response of the spin to the external field de- region of low temperature below 141.0 K)
SU Yuling et al., Magnetic properties of rare earth HoCrO3 chromites 1063

Fig. 5 Ac susceptibility M' as a function of temperature at frequen- Fig. 6 Isothermal magnetization vs. temperature curves at different
cies f=199, 987, and 3987 Hz, respectively (The insets give the temperatures 10, 30, 120, and 160 K for HoCrO3 sample (The
local zoom for the eyes at two peaks near 141.0 and 7.5 K) inset is the FM contribution vs. magnetic field H at 60 K)

glass (SG) phase, cluster glass phase, FM and AFM phase Fig. 7 displays the specific heat capacity (Cp) of the inves-
and so on. For these, we give the local zoom for two peaks tigated HoCrO3 sample, plotted in steps of 1 K around 10 K
near TN1 and TN2 in the inset (a) and (b) of Fig. 5. It can be and 140 K to confirm the magnetic data. We have measured
seen that, near TN1, either in peak height or in peak tempera- the sample in a zero-field state and with an external applied
ture position, no change is observed, indicting that the ac field of 9 T. It can be seen that a Ȝ-like anomaly peak is ob-
susceptibility peak is frequency-independence near TN1. This served with the maximum at TN1=141 K, indicative for the
excludes the possible existence of spin-glass and cluster Néel temperature of the magnetic ordering of the Cr mo-
glass phase near TN1. Combining Fig. 2 and earlier related ments, and the peak is depressed and broadened smoothly
work by other researchers[28], the present peak near TN1 with the magnetic field increasing. Owing to the suppression
shows the magnetic transition from PM phase to CAFM and of the magnetic fields on the thermal disturbance, the asso-
FM phase. In other words, there is a coexistence of CAFM ciation among magnetic moments is dominant above TN1,
and FM phase below TN1=141.0 K. As to the peak near TN2, and the magnetic order fluctuations appear. With the tem-
except the change in peak height, no changes in peak posi- perature decreasing, the association between magnetic mo-
tion can be observed, either. This should be caused from the ments gradually increases. As the external magnetic field
combined effect of the isotropic Cr3+-Ho3+ and Ho3+-Ho3+ strengthened, the Ȝ-like peak is depressed and broadened
interactions. The isothermal magnetization loop at different smoothly, the magnetization curve changes gradually around
temperatures will be meaning to understand the magnetic TN1. Between 30 and 100 K, there is no anomaly in the Cp
characteristics of heavy rare earth HoCrO3 chromites. Fig. 6 data. This fact may indicate that the global antiferromagnetic
gives the isothermal M-H loops at several characteristic structure (Ƚ2) does not change below TN1. And there is no
temperatures 10, 30, 120 and 160 K. Obviously, below TN1, hint for long-range ordering of the holmium magnetic mo-
several loops are well symmetrically closed with square-like ments. Moreover, we also note that there is a shoulder-
form, but not magnetic saturation, which originates in shaped anomaly below 7.5 K in the specific heat capacity
CAFM and FM properties. Furthermore, the dc magnetiza-
tion M increases linearly for all the loops in the region of
larger magnetic field. This kind of magnetization loop and
its linear change at high temperature is also attributed to the
coexistence of FM and CAFM state. Therefore, the
high-field part of the M(H) evolution can be represented as
M(H)=ȤAFH+ıs, where ȤAFH is the antiferromagnetic contri-
bution and ıs is the saturation magnetization of the weak
ferromagnetism[29]. The value of ıs is obtained by the ex-
trapolation of the linear part of M-H curve to zero. In addi-
tion, the FM contribution for HoCrO3 can be, thus, obtained
as shown in the lower inset in Fig. 6 by subtracting the AFM
contribution from the total magnetization (T=60 K). Above
Fig. 7 Temperature dependence of the specific heat capacity under
TN1, the hysteresis apparently disappears at 160 K, indicating
zero and 9.0 T magnetic field (The inset shows the tempera-
that phase transition from canted antiferromagnetic to para-
ture derivative Cp/T and d(Cp/T)/dT vs. T and the transition
magnetic occurred below 160 K, i.e. a linear increase in the
temperature is indicated)
magnetization.
1064 JOURNAL OF RARE EARTHS, Vol. 29, No. 11, Nov. 2011

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