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Shubnikov-de Haas Oscillations in New Organic Conductors (ET)8[ Hg4Cl12(C6H5Cl)2] and (ET)8[
Hg4Cl12(C6H5Br)2]
R. Lyubovskii, S. Pesotskii, A. Gilevski, R. Lyubovskaya
To cite this version:
R. Lyubovskii, S. Pesotskii, A. Gilevski, R. Lyubovskaya. Shubnikov-de Haas Oscillations in New Or-
ganic Conductors (ET)8[ Hg4Cl12(C6H5Cl)2] and (ET)8[ Hg4Cl12(C6H5Br)2]. Journal de Physique
I, EDP Sciences, 1996, 6 (12), pp.1809-1818. �10.1051/jp1:1996189�. �jpa-00247282�
J.
Phys.
I France 6(1996)
1809-1818 DECEMBER1996, PAGE 1809Shubnikov-de Haas Oscillations in New Organic Conductors
(ET)8[Hg4C1i2(C6H5Cl)2j and (ET)8[Hg4C1i2(C6H5Br)2j
R-B-
Lyubovskii
(~~~~*), S-I- Pesotskii(~,~),
A. Gilevski(~) and
R-N-Lyubovskaya (~)
(~) Institute of Chemical
Physics
atChernogolovka RAS, Chernogolovka,
Moscow region, 142432 Russia(~) International Laboratory of
High Magnetic
Fields and Low Temperatures, 53-529 Wroclaw, Poland(Received
5April
1996,accepted
iiJune1996)
/
PACS.74.70.Kn,
Organic superconductors
PACS.72.15.Gd
Galvanomagnetic
and other magnetotransport effectsAbstract. Trie results of trie
investigations
of Shubnikov-de Haas oscillations in trie quasi- two-dimensionalorganic complexes (ET)s [Hg4C1i2 [C6HSX)2],
where X = Cl, Br in triemagnetic
fields up to 40 T
were reported. These results allow
one to obtain some information about Fermi surface in trie mentioned
complexes.
Shubnikov-de Haas oscillations in triecompound
with X
= Cl
correspond
at least to two differentcyhndrical
sheets of Fermi surface with trie cross-section in(bc)-plane
of13% and 20% Brillouin zone cross-section. Shubnikov-de Haas oscillations m trie complex »ith X = Brcorrespond
to onecy.hndrical
sheet ~vith trie cross- section in(bc)-plane
of13% of Brillouin zone cross-section. Trieexperimental
results for triecomplex
~vith X= Br more agree with the theoretical calculations of Fermi surface than for trie
complex
~vith X= Cl
Introduction
In trie fate 80ies the
family
ofquasi-tn<-dimeiisional
organicsuperconductors
based on bis-(ethylenedithio)tetrathiafulvalene (ET)
~N.as filled upby
two newsuperconductors
withpoly-
merized halomercurate orrions,
namely (ET)4Hg2_78C18
and(ET)4Hg2 898r8
withTc
= 1.8 K
and 4.3 h.
respectively il, ii.
Trie work n~ith trie anions of this type seemed to be promising due to trie unusualproperties
of triesuperconductors.
Inparticular,
a record value of triederivative of trie Upper critical field
dHc2/dT
m~ 10
T/K along
trieconducting
sheetsregis-
tered in
(ET)4Hg2 sgBr8
at arelatively
low criticaltemperature,
leads to a record excess ofa
paramagnetic
bruit in organicsuperconductors
[3].Besides,
an unusualgrowth
of criticaltemperature
n>ith an externat pressure noncharacteristic of normalsuperconductors
was ob- served in thiscompound
at a pressure up to 3-5 kbar [4]. Trie electron structure of thesecompounds
was ofimportance,
however its detailedinvestigation
withusing
amagnetic
fieldwas restricted
by
an internai randompotential
inherent in thesecompounds,
which results intrie value ~dT « 1 in trie total range of
really existing
fields. Such apotential
is a result of that(*)
Author forcorrespondence le-mail: rustem©icp.ac.ru)
©
LesÉditions
de Physique 1996Hg
atoms form their own sublattice in(ET)4Hg2
78C18 and(ET)4Hg2.898r8 single crystals
which is incommensurate with trie lattice of trie basic matrix
[5].
Therefore it isquite
rea-sonable to
synthesize
trie conductors with halomercurate aurons without a randompotential.
This
opportunity
was realized in triesynthesis
of afamily
of isostructuralorganic
conductors(ET)8(Hg4C1i2(C6H5Cl)21 II), (ET)8(Hg4C1i2(C6H5Br)2] (II), (ET)8(Hg4Br12(C6H5Cl)21 (III)
and
(ET)8(Hg4Br12(C6H5Br)2] (IV)
[6]. Triecrystal
lattices areregular
in these salts ~N.hichare metals at room temperatures
I?i.
However III and IV become dielectrics below 90 K and 160K, respectively.
Il is characterizedby
a weakgrowth
of trie resistance below 10 K andonly
I
keeps
a metallic behaviour down to 1.4 Ii [8].Trie
magnetoresistance
of trie salt I denoted below as(Cl, Cl)
and that of trie salt II, denoted below as(Cl, Br)
was studied in this work. Wereported
earlier about trie observation ofShubnikov-de Haas
(SdH)
oscillations in thesecomplexes [9, loi.
Trie present work exhibitsmore detailed
investigations
of SdH oscillations and first of all trie detailedcomparative analysis
of SdH oscillations in triecompounds (Cl, Cl)
and(Cl, Br)
and their Fermi surfaces(FS).
Experimental
The
objects
understudy
were triesamples
of(ET)8(Hg4Ch2(C6H5Cl)21 single crystals
which appear asirregular parallelepipeds
with I.o x I.o x o-1mm3
characteristic sizes. Trie totalX-ray analysis
of thiscompound
made at roomtemperature
is described in[îj. (Cl, Cl) single crystals
bave alayered
structureanalogous
with that of trie other ET-based conductors. ETloyers
are located in(bc) plane.
All ET molecules areparallel
to each other in trielayer
thatis characteristic of
p-type packing.
ETlayers
alternatealong
a* direction and areseparated by polymerized [Hg4C1i2(C6H5Cl)~~]
anions. Trie unit cell is triclinic with Z= 1 and contains 8 ET molecules per cell.
(Cl, Br) complex
is isostructural to(Cl, Cl)
one. Trieconductivity
of both salts in
(bc) plane,
i e. in trieplane
of ETloyers
constitutes s= 10
S/cm
and thatbetween trie
loyers,
1.e.along
a* direction, is 3-4 orders lower. Trietemperature dependence
of trie resistance for(Cl, Cl) complex
is metal-like without anypeculiarities
within 1.4-300 K at triemeasuring
current I j(bc).
At trie same direction of trie current a weakgrowth
of trieresistance was observed below 10 K in
(Cl, Br) complex
[8].Magnetoresistance
measurements were carried ontby
using a standardfour-probe technique
at an
alternating
current of 330 Hz. Both alongitudinal
resistance at I j(bc)
and a transverseone at I j a* were measured. For
measuring
amagnetoresistance
amagnetic
field up to 15 Twas
generated by
asuperconducting
solenoid and that upto_40
T wasgenerated by
apulse
solenoid.Only
in trie case of asuperconducting
solenoid one could rotate asample
varying itsorientation in a
magnetic
field. SdH oscillations of trie resistance found in these measurements wereanalyzed by using
a standard method of fast Fourier transform(FFT).
Results
Figure
1 shows trie fielddependence
ofmagnetoresistance
for(Cl, Cl) single crystals
at field directionperpendicular
to(bc) plane
and at current directionalong
thisplane.
SdH oscillationsare observed even at î-8 T and appear as almost an ideal sinusoid with 250 T
frequency.
FFTof this curve
(see
insert A inFig. 1)
confirms this factdemonstrating
a very weak contributionof trie second harmonic. However at trie same field and current directions trie contribution of SdH oscillations with
higher frequencies
growsquickly
in trie fieldshigher
than 15 T(pulse
fields up to 40
T) (see
insert B inFig. 1).
Trie presence of SdH oscillations with other
frequencies
can be also observed in trie fieldsup to 15 T but in trie conditions distinct from those
presented
inFigure
1.Figure
2displays
SdHN°12 OSCILLATIONS IN NEW ORGANIC ET-SALTS 1811
6.5
6.0
5.5
B
£
5.0 TJZ
O
ç/
4,5A
~
4.0
t
(
3.5
~
3.0
1o i
,
T
Fig.
l. Shubnikov-de Haas oscillations m triesingle crystal
of(ET)8[Hg4C1i2(C6H5Cl)2]1
Hjj a*,
trie current I is
parallel
to trie bcplane
and T= 1.45 K. Insert A:
amplitude
of fast Fourier transform for the oscillationspresented
inFigure
1. Insert B: Shubnikov-de Haas oscillations in apuise field;
H
jj a*, the current is
parallel
to the bcplane
and T= 1.45 K.
oscillations at current direction I
jj a* and at ç2 = 25°
,
where ç2 is trie
angle
between trie field direction and trie direction a*(~
= o at H
jj
a*).
FFTrepresented
in trie insert toFigure
2 indicates that trie curve shown in trieFigure
is asuperposition
of SdH oscillations of at least rivefrequencies.
Figure
3 shows SdH oscillations in(Cl, Br) single crystal
at trie direction of trie measuring current I j a* and at H j a*. These oscillationstogether
with their Fourierspectrum (see
trie insert toFig. 3)
are similar to those observed for(Cl, Cl) samples
at trie same field direction.Moreover,
triefrequency
of SdH oscillations(F
= 235
T)
in(Cl, Br)
is close to that of trie oscillations found in(Cl, Cl)
at Hjj a* and I j
(bc). However,
in contrast to(Cl, Cl)
FFTyields only
onefrequency
of SdH oscillations in(Cl, Br) crystals
at ail orientations of amagnetic
field
(trie
contributions of trie otherfrequencies
orhigher
harmonics are rathersmall).
Trie
angular dependence
of SdHfrequency
was studiedquite
in detail in a wide range of trieangles
ç2 = +70°. Trie results of trie measurements are shown inFigure
4 inpolar
coordinates for(Cl, Cl) samples
and inFigure
3(see
insertB)
for(Cl, Br)
ones. Triefollowing peculiarities
of these measurements should be noted:1)
SdH oscillations are characterized in(Cl, Br) by
trieonly frequency,
whoseangular dependency
appears as astraight
lineperpendicular
toa*;
2)
in(Cl,
Cl SdH oscillations are characterizedby
sixfrequencies
whoseangular dependence
are also more or less
correctly
describedby straight
hnesperpendicular
toa*; 3)
at H j a*trie values of these
frequencies
constituteFi
" 150
T, F2
" 250T, F3
" 400
T, F4
" 500
T,
0.2
O.1
~
O.O
(
-0.1~
d e
~'
(
fÎÎ
-0.2 ~Î
S-0.3
H,
-0.4
O.lO 0. 0.12 0.13
/H, /T
Fig.
2. Shubnikov-de Haas oscillations in thesingle crystal
of(ET)8[Hg4C1i2(C6H5Cl)2]
after a subtraction of theregular
part where ~J=
25°,
trie current is Ijj a* and T
= 1.45 K. Insert:
amplitude of trie fast Fourier transform for the oscillations presented in
Figure
2.F5
" 650 T andF6
" 910 T,
respectively (this
is trie result of trieinterpolation
of trie hneardependencies
inFig.
4 on trie field direction H j a*); 4)
trie contribution of oscillations of eachfrequency
to trieresulting
oscillation curveessentially depends
on ç2 and current direction in(Cl, Cl).
At I j
(bc)
trie oscillations withF2 frequency
dominatesignificantly
at almost allangles
ç2. Trie contribution of SdH oscillations with other
frequencies
is notlarge,
moreover trie oscillations withFi
andF6 frequencies
were not observed at anyangle
ç2. At I j a* SdH oscillations withF2 frequency
dominate as well. However for most ç2values, especially
ifthey
are not close to ç2 =
o°,
trie contribution of oscillations with otherfrequencies
issignificant
and even
compatible
with that of trie mainfrequency F2 (see
trie insert inFig. 2).
Trie fact that under certain conditions trie contribution of SdH oscillations in
(Cl. Cl)
is madeonly by
trie mainfrequency F2,
enables trie evaluation ofcyclotron
mass of trie carriersassociated with trie oscillations of this
frequency.
Trie insert inFigure
5 shows trie temperaturedependence
oflogarithm
of trie reducedamplitude
of SdH oscillations at I j(bc)
and ç2= o°.
Trie
dependence
is wellapproximated by
astraight
hne within trieexperimental
error. Thusone can use a standard
relationship
for trie evaluation of acyclotron
mass:In(À/T)
= const
2~~ckBm*(T TD)lehH Il)
where A is an oscillation
amplitude,
m* is acyclotron
mass, TD isDingle temperature.
Trie evaluationyields
m*= 1.35 mû
N°12 OSCILLATIONS IN NEW ORGANIC ET-SALTS 1813
11
~ B
Î
1
HJn.
0f
A
E
W
OE E
<
t~
H,T
4 14 16
H, T
Fig.
3. Shubnikov-de Haas oscillations in triesingle
crystal(ET)8[Hg4C1i2(C6H5Br)2]
with triefield orientation H
ii a* and temperature T
= 1.45 K. Insert A: FFT for trie oscillations
displayed
in thefigure,
msert B:angular dependence
of the frequency of Shubnikov-de Haas oscillations inpolar
coordinates.
The insert in
Figure
6 shows that trieapplication
of trierelationship Il)
to SdH oscillations in(Cl, Br) complex
isquite
correct. Trie evaluation of acyclotron
mass in thiscompound yields
m*= 1.25 mû which is close to trie
analogous
one in(Cl, Cl).
Figures
5 and 6 exhibit trieangular dependences
of trieamplitudes
of SdH oscillations of trie mainfrequency F2
in(Cl, Cl)
at Ijj
(bc)
and those of triefrequency
F in(Cl, Br)
at Ijj
a*, respectively.
Trieamplitudes
of oscillations bave a maximum in bothcompounds
which does trot coincide with trie direction H j a*. Trieamplitude
becomes almostequal
to zero in eachcompound
at ç2 > +60°. Besides trie intermediate minima ii which trieamplitude
is close tozero, are
quite
ofimportance.
These minima appear at trieangles
ç2 = +28° for(Cl, Cl)
andat ç2 = +35° for
[Cl, Br).
Discussion
The
analysis
ofX-ray
data I?i enabled one to calculate a zone structure of(Cl, Cl)
salt[11].
Its unit cell contains 8 donor ET
molecules,
therefore trie interaction between 8highest
oc-cupied
molecular orbitals(HOMO)
results in trie formation of 8 energy zones.According
to a stoichiometric formula each ET molecule bas 1.5 electron in trie unit cell and therefore 12 electrons are to bepopulated
at 8 energy levels. Trie system understudy
may be either a two-dimensional semiconductor or a two-dimensional metaldepending
on triedegree
of trieHia* j
§
+
5°° T 250
THla*
Fig.
4.Anglular dependence
of triefrequencies
of Shubnikov-de Haas oscillations in(ET)8 [Hg4C1i2(C6H5Cl)2]
mpolar
coordinates.overlapping
or trieavailability
of trie energy gap between trie 6th zone and trie 7th one. Trie calculations [11] showed that there is a smalloverlapping
between these zones which defines theirpartial occupation by
electrons andconsequently
a metallic behaviour ofconductivity
of this salt down to heliumtemperatures.
Trie calculated Fermi surface(FS)
was found to consist of twocylinders
whose axes areparallel
to a*. Trie cross-section of thesecylinders
in bcplane
is shown in
Figure
7. Trie calculationsyielded
trierigorously equal
values for trie areas of trie sections for thesecylinders
which constitute13%
of trie area of acorresponding
section of trie first Brillouin zone. However triecylinder
A is associated with electrons as carriers and triecylinder
B is associated with holes. It is stated in[11]
that these closed FSappeared
as a result of triehybridization
of two hidden one-dimensional FS. One couldexpect
quantum oscillationsonly
with triefrequency
of about 250 T at H j a* from FS of such ashape (not considering
trie
possible
contribution of trie harmonics andmagnetic
breakdownorbits).
These calculations are
qualitatively
andquantitatively
inagreement
with trieexperimental
data on SdH oscillations in(Cl, Br).
Trieangular dependence
of triefrequency
of SdH oscil- lationsapparently
enables trieimagination
of FS in thiscompound
as onecylinder (or
severalcylinders
withequal
areas ofcross-sections)
with trie axis directedalong
trie direction a*. At H j a* triefrequency
of SdH oscillations is 235 T that is close to trie calculated value.A
significantly
morecomphcated
case is for
(Cl, Cl) compound
for which trie calculation of FSwas made
il ii.
Triestudy
of SdH oscillations at various field andmeasuring
current orientations revealed trie existence of oscillations with six differentfrequencies.
All thesefrequencies
bave triedependences
on trieangle corresponding
to triecylindrical
sheets of FS(see Fig. 4).
Howeveronly
a part of themcorresponds
toreally existing
closed orbits. Itobviously
follows from triefact that trie sum of all
frequencies
is more than triefrequency corresponding
toloo%
of trie first Brillouin zone. One can see that allfrequencies
are a hnear combination of twofrequencies Fi
andF21 F3
"
Fi
+F2, F4
"
2F2, F5
"
Fi
+2F2
andF6
"
Fi
+3F2. Figure
4 demonstratesthat trie
frequency Fi
is observed in a very narrow range of trieangles,
at trie same timeN°12 OSCILLATIONS IN NEW ORGANIC ET-SALTS 1815
200
f~
ÎÎ
il, Ko -ioo
~tJo
Fig.
5.Angular dependence
of theamplitude
of Shubnikov-de Haas oscillations at the fundamental frequency F2 mJET)8[Hg4C1i2(C6H5Cl)2]
singlecrystal
when current isparallel
to the bcplane
and T
= 1.45 K. Insert: temperature
dependence
of the reducedamplitude
of Shubnikov-de Haasoscillations at the basic
frequency
F2.trie
frequency F3
appears at FFTsignificantly
morefrequently.
Therefore we suppose that triefrequencies F2
andF3 correspond
to trie real closed orbits. Triefrequency F4
is mostprobably
trie second harmonic ofF2.
Trie otherfrequencies
areprobably
so called combinedfrequencies: Fi
=
F3 F~, F5
=F3
+F~, F6
=F3
+2F2,
which can arise forexample
due to amagnetic
interaction[12].
It also cannot be excluded that triefrequency F5
is associatedwith the
magnetic
breakdown orbit. Thus SdH oscillations show trie existence of at least two differentcylindrical
FS sheets in triecomplex (Cl, Cl)
which have the cross-section in bcplane equal
to13%
and20%
of trie first Brillouin zone cross-section andcorrespond
to triefrequencies F2
andF3.
However a more detailedinvestigation
will beenough
to confirm this fact.Trie
following problem
is not alsoquite
clear: how manycylindric
sheets of FS which possess trieequal
areas ofcross-sections,
areresponsible
for trie oscillations with trie mainfrequency F2
in(Cl, Cl)
and for trie oscillations with triefrequency
F in(Cl, Br). According
to trie theoretical calculations of FS for(Cl, Cl) [11]
one can expect that twoFermi-cylinders
with trieequal
areas of cross-sections in everycompound contril~ute
to trie oscillations with thesefrequencies.
In this case trierelationship (1)
for trietemperature dependence
of trieamplitude
of SdH oscillations is validonly providing
that both in(Cl, Cl)
and(Cl, Br) Fermi-cylinders
~&.ith
equal
areas are associated with the carriers which baveequal cyclotron
masses. It is seen from the inserts inFigures
5 and 6 that therelationship (1)
holdsquite
well for bothcomplexes.
Therefore the conclusion may be drawn that either the contribution to SdH oscillations with
80
/~
é
~
60
Jà à
~
K
m a lJ1
o
ù20
E
-i
angle (~£J°)
Fig.
6.Angular dependence
of theamplitude
of Shubnikov-de Haas oscillations m(ET)8 [Hg4C1i2(C6H5Br)2]
at the T = 1.45 K. Insert: temperaturedependence
of the reducedamplitude
of the oscillations with the field orientation Hjj a*.
/~S/~fi~~
z
a
~~li~/S~~
Fig.
î. The cross-section of Fermi surface m the bc plane m(ET)8[Hg4C1i2(C6H5Cl)2]
at roomtemperature
Ill].
N°12 OSCILLATIONS IN NEW ORGANIC ET-SALTS 1817
the
frequency F2
in(Cl, Cl)
and thefrequency
F in(Cl, Br)
is madeby only
onecorresponding Fermi-cyhnder
in eachcomplex,
or such a contribution is realizedby
severalcylinders
whichare characterized
by equal
areas of cross-sections andequal cyclotron
masses of the carriers.This is confirmed
by
trieangular dependences
of trieamplitudes
of SdH oscillations with triefrequency F2
in(Cl, Cl)
and triefrequency
F in(Cl, Br) represented
inFigures
5 and6, respectively.
Bothdependences
arequite
similarqualitatively. They
both are characterizedby
incoincidence of trie maximum of trieamplitude
with trie direction of trie field Hjj a*.
This incoincidence is associated
probably
with a lowsymmetry
ofcrystal
lattice of triesamples
studied. Both
dependences
demonstrate trie intermediate minima of trieamplitude
which trie mostprobably
arise because of aspin splitting
of Landau levels.Keeping
thissplitting
in mind one can introduce a
lowering multiplier
in trie expression for trieamplitude
of SdH oscillations [12]cos(~gpm* /2mo)
where p is harmonic's number and g is
g-factor.
It is reduced to zeroproviding
thatgpm* /mo
# 2n + 1
where n is an
integer. Considering
that acyclotron
massdepends
on ç2 as trie areaenveloped by
trie
corresponding orbit,
1.e.m*(ç2)
=m*(o)/
cosç2 andtaking
into accountm*(o)
=
1.35mo
obtained earlier for(Cl, Cl)
andm*(o)
=
1.25mo
for(Cl, Br),
one obtains that at g = 2 trieamplitudes
of trie first harmonics of SdH oscillations withF2
and Ffrequencies
vanish atn = 1 and ç2
= +28° and ç2 = +34°
respectively,
that agrees well with trieexperimental
results obtained for bothcomplexes (see Figs.
5 and6).
It is obvious that triesuperposition
of SdH oscillations withequal frequencies
but differentcyclotron
masses couldhardly
enable one to observe such very well resolvedpictures
of"spin
zeros" which were found in(Cl, Cl)
and(Cl, Br).
Conclusion
The
study
of trie behaviour of SdH oscillations in trie isostructuralorganic
conductorsETB [Hg4Ch2(C6H5Cl)21
andETB(Hg4C1i2(C6H5Br)21 permitted
one to obtain triepreliminary
vi- sualization on FS in thesecompounds.
InETB(Hg4C1i2(C6H5Br)21
it consists of one or severalcylindrical
sheets with trie axes directedalong
a* and trieequal
areas of cross-sections constitut- mgapproximately
13To of trie area of triecorresponding
cross-section of trie first Brillouin zone in(bc) plane.
InETB(Hg4Ch2(C6H5
Cl)2] FS trie mostprobably
contains at least twocylindri-
cal sheets with different areas of cross-sections
constituting approximately 13%
and20%
of triearea of trie cross-section of trie first Brillouin zone in
(bc) plane.
ForETB(Hg4Cl12 (C6H5Br)21
trie data obtained are in a
qualitative
andquantitative agreement
with trie theoretical calcu- lations of FS whereas trie results obtained forETB(Hg4Ch2(C6H5Cl)21
areonly partially
inagreement
with these calculations.Acknowledgments
The authors express their
gratitude
to V.I. Nizhankovskii for bishelp
in trieexperiment,
to A.E. Kovalev and M.V. Kartsovnik for triehelp
in trie treatment of trieexperimental
data and fruitfuldiscussion,
to Ya.Klyamut
and E-B-Yagubskii
for triesupport
of this work. Trie workis
supported by
trie Russian Foundation of FundamentalInvestigations (93-02-2384),
INTAS(93-2400)
and TSF(JB 3100).
References
iii Lyubovskaya R-N-, Lyubovskii R-B-,
ShibaevaR-P-,
AldoshinaM.Z., Goldenberg L.M.,
Khidekel'Mi. andShul'pyakov Yu.F.,
JETA Lett. 42(1985)
468.[2]
Lyubovskaya R.N., Zhylaeva E.I., Zvarykina A.V.,
LaukhinV.N., Lyubovskii
R-B- and PesotskiiS-I-,
JETA Lett. 45(1987)
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