Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br)
Second order phase transition, observed previously in the title salts in thermal expansion studies close to 80 K, was studied in insulating X= Cl and I salts by a transient spectroscopy of structural relaxation and by controlled annealing. A notable difference in the activation energy of transformat...
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| Дата: | 2001 |
|---|---|
| Автори: | , , , |
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| Мова: | Англійська |
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Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine
2001
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Репозитарії
Surface| _version_ | 1869291151594356736 |
|---|---|
| author | Tanatar, M. A. Ishiguro, T. Kushch, N. D. Yagubskii, E. B. |
| author_facet | Tanatar, M. A. Ishiguro, T. Kushch, N. D. Yagubskii, E. B. |
| author_institution_txt_mv | [
{
"author": "M. A. Tanatar",
"institution": "Інститут хімії поверхні НАН України"
},
{
"author": "T. Ishiguro",
"institution": "Japan Science and Technology Corporation"
},
{
"author": "N. D. Kushch",
"institution": "Institute of Problems of Chemical Physics"
},
{
"author": "E. B. Yagubskii",
"institution": "Institute of Problems of Chemical Physics"
}
] |
| author_sort | Tanatar, M. A. |
| baseUrl_str | |
| collection | OJS |
| datestamp_date | 2018-11-27T09:42:39Z |
| description | Second order phase transition, observed previously in the title salts in thermal expansion studies close to 80 K, was studied in insulating X= Cl and I salts by a transient spectroscopy of structural relaxation and by controlled annealing. A notable difference in the activation energy of transformation and in annealing behavior compared to the metallic X= Br salt was found, showing transformation towards different structural states at low temperature.
  |
| first_indexed | 2025-09-24T17:25:26Z |
| format | Article |
| fulltext |
TRANSIЕNT sPЕс'rRoSСoPY oF 80 K sЕCoND ORDЕR
PIIASЕ TRAN sITIoN IN K- (BЕDT.TTF)2С u tТ.{ (сlt{)2] х
(Х= Cl, I' and Br)
М.A.Tanatar'-3, T. lshigu ro2,з, N.D. Kushсha, and Е.B.Yagubskiia
.Institutе,of S.fк:fJ:r;r-)ff t}?Li,..1Ж'?fj.ienсе*
2Dеpartmеnt
",
*n,]'.,, iiу"i"Ъы".i''iiу, s uкуo-iu, Kуoto 606-8 5 02' JAPAN
1;:;;{i:{tt1i.'-t',ъH*i-.*}'difliх**+:т,,^,;lf ''3;Jl,*
oo..."Ъ.."ond
ordеr phasе tгansiti"n. 1P.,,.T..9.::::l::'у='}''l;
.'.'. salts in thеrma,l
ехрansion studiеs.ro,.uio вЪ K';;;siudied r" иJ"йii"* i: С1.and I salts bу a transiеnt
*oЬ"t,osсopу oг,t.сtu,ui,.lu*uiion and bу
"o".,oii.J.u"йaling
A notablе diffегеnсе in thе
йivatiоn еnеrgу ",.,."-r",*",i""
;i1
ll.:::,.;t;*
behavior сomP::."o .o thе metalliс Х= Bг
salt *,as found, showrng tгansformation towaгds dltТегеnt stгuсtuгal statеS at low tеmperaturе.
Introduсtion -тгr г.'гхrl/ГIrT\.lY |-BЕ,DT-TTF. or Е.l
.
Salts of к-(BЕDT-TTЕ)zCuГN(CN):]Х ..tBЕDl-:TЕ
or ЕТ
'
bis(еthуlеnеdithio;tеtratьL-iiiЬ.,
'=Ъ],Ь,t"iо,i,
*. abbrеviatе thе salts bу thеir Х in thе
following] foгm a ,"",Ы;?;;;l*l::l:::#;'-1"'::"..':llРii"RJ#.:"ij:.i:-::".,
il'в к iiЪr salts at u*ьi.n'and 0'3 kbч pl.:i}l..;lъffi"il?.ui' i;l";;;i. rеallу. shows
н*;r:*il-'ll""''".,ilT:.J;:"ixj+}gi*Ёt j:#i:;'[,}ж:,":i,:"3..!"ц'
,i"'й,ututo.' -u,.u*J,u#;;ж"11"*'l i;::*.*1}'Тt i:H"'i:Ti^i:lж"}Ъ.:.i:
lopri."tion of hуdrostatiс pressure^abo"9- Y;,.,Т''"il;;,;';;;;"Ъ ЁT molесulе [2]
?:J#Tъl#i:j:.""'::"jЁ"lгн;:1жТJJ.i:ж-'T:!i:iii,.;;';;illhе thrее salrs
сonformationur аi.o,а"Т iioЬ,"*.d'ut ."""' ,;й;;;tu,e, *ьit" thе statе at low tеmpеraturе:
seеms to bе ditrеrеnt [2] }P{o.. oi,.jь-iй"._oi есlipsеd €) and staggегеd (S
сonfoгmations of втluas}]unа ln l satt at izт к *l,t' avегagе popu'ation of appгoximatеl.'
0'67 and O'33, геspeсti'"lу tzl In Cl and-Br,,"i', 'ь" 'i*ation
is more сontгoveгsial. Initialll
itwasсonсludеdthatеthуlеnе*:""p1:::.;,"j.i"в-.onformationalrеadуatI21K|2.'
Howеvеr, rесеntlу thе suрЪrstru..u." .hu.,u"i.i"i".l.п1g':]"r::J:: xj}:iJ}:]#ц.!
16l sa'ts *u, аi,"ou"',.ji"","'"L".d in.l:г^cе thегmal faсtors ",."Ъъ:;;;.;o.к ,uь.ьrЬ"ь..
i;j
"t1-,.";;;,Ьnь.',.йуЁl^...:9.'l1чL7,Ц Pгoсееds bеtwееn'^l ;;';-;'l mеtalliс ste:.
of phasе transltlon "
Ъo?rsl Thе transformation pгomot.-''1" 'oilij;;й;';;;;;i1i:...
in Ьг salt with both "йiвi
Ьolесulе.and with the moleсulе. in' whiсh еight hуdгog.l. lt: -
aге сomplеtе,, ". йЁьji,.,uЬui*..а ъy ;;;;;;;; (о-вг'.satt.in thе following) LlU-l:
Sinсе thе аir",enс"ln к1t)b*,*..":"l^.dъ,;;;,; *'е1l as bеtwееn Cl salt in mеtall:-
and insulating statеs, appеar.s.сlose l:]ч:J;d;'".;й
Гiur,."'^.:1o. thought that namеlу t':.
1 aсk o f
", 9 : " :* .', .l::lТ:' T
jt
Л r ч**."''
.l'н;
5;ж "l,i j LТ' i:Н жl:
:ij;ж' ; :; * :":: ж,
ig
:, jl&
:::: т:i:: i l1i E ll*l i :r iЪЧ Тli i l lj,], . l
,utti'вoк(вrsati;and84K(Isalt)t*""'.t.,ioiьl'fеaturеas.80Ktгansitlon,lnt:
l)о
DЕR
l]х
. ..1
ill
:n thеrmal
: tгansiеnt
:е:.се in thе
:"..iс X= Br
:]-]егatuге.
г-1 ls
rl: Х in thе
( .n Br and
s ] struсtural
:: .1' shows
1 зrd I salts
:: statе by
в: :.g duе to
Е ::.гее salts
:::'еratuгеs
eЁ:эгеd (s)
щ. - хimatеlу
r: Initiallу,
^a t, r411 -,', l\ lzl
г
.-
:] and Cl
п ...-;aу
data
s.:.Эгanсhes
ше::]liс statе
й: -еn atoms
ш: [10-15].
A . mеtalliс
l .:пrеlу thе
}i ,3 statеs'
; -- r found
.3 K (Сl
- in this
aгtiсle)' In view of rесеnt rеsults foг Bг salt, it was of intеrеst to study thе геlation bеtwееn thе
80 K transition in mеtalliс and insulating (Cl and I) mеmbеrs of thе йmily
We addгеssеd th.is quе_stion bу studying (l) thе еffесt of annealing in thе viсinity оf
thе 80 К tгansition on Сl and I сompounds, siйilaг to Br and D-Br salts 1я-ls;, and (zf thе
tеmperatuгe dеpendеnсе of thе struсtural геlaхation timе' similaгto our studу oгвr. unj о-в,
salts [9] Thе study is based on a сhaгaсtегization of thе isоthегmal rеsistanсe tгansiеnt R(t)
1nфсеd by thегmal
"y"]11ч
and сontrolling R(T) as a гesult of annеaling. Large hystегesl, Ьt
R(T) in Bг and Cl salts [t7] g1vе a largе magnitudе of thе tгansiеnt at a fiхеd йmpЬгaturе. No
hysterеsis was notiоed-in I sаlt in pгеviоus mеasurеmеnts Il9]. Сontrary to this obseгvation,
spесial isothermal studiеs in this woгk геvеaled rеsistanсе iеlaхation in I salt in 100 to 60 K
rangе, but a small magnitudе оf thе tгansiеnt (геlativе геsistanсе сhangе in l0.з to l0{ rengе,
approхimatеly two ordеrs of magnitudе smallег than in Bг and Cl silts) pгесludеd Ггоm]ts
dеtailеd сharaсtеrization. Hеnсе, in the disсussion of геlaхation data *. Ь.u, only on Cl salt
in соmparison with Bг and D-Bг salts [9]
As a геsult of this studу wе show that annеaling of Cl and I salts in thе viсinity of thе
sесond ordеr 80 K transition doеs not lead to a gradual tгansfoгmation towards any nеw statе.
Wе rеlatе this diffеrеnсe in annеaling еffесt сomрarеd to thе Bг and D.Bг ialts with a
pгofound diffегеnсе in the tеmpегaturе dеpеndеnсе of struсtuгal rеlaхation timе bеtwееn СI
and Br salts. This struсtural diffеrеnсе is intегpretеd as duе to transfoгmation tоwaгds
сiiffегеnt statеs of еthуlеnе oгdегing in Сl and Bг salts in thе ground state' We disсuss a
рrеssuге-tеmpеratuге phase diagram of thе 80 K transition in thе viсinity of mеtal - insulatoг
boundary in pгеssuге in thе fraп,rеwoгk of сompеtition bеtwеen supегstRlсturе sub-phasе аnd
ordегing tгansfoгmations.
Тransiеnt spесtrosсo p}'
Duгing struсtuгal геlaхation thе systеm movеs fгоm an ехсitеd statе, сгеatеd
aгtifiсiallу or natuгallу, towaгds a stablе statе. Тhis сhangе has its own aсtivation еnегgy Е
and is ехponеntial in timе, with a геlaхation timе т following Aгrhenius law, provided that thе
systеm сan bе trеatеd as having two disсrеtе еnеrgy lеvеls [2O],
т:тgeхp(ЕikT) (l)
т0 сan vary in a bгoad гangе, dеpеnding on the phуsiсal oгigin of thе pгoсеss. Struсtuгal
гelaхation сan be studiеd by mеasuгing сhange in timе of anу of thе physiсal propеrtiеs G(t,T)
of сompound, whiсh in сasе of ехponеntial геlaхation follоws thе low
с (t)-с (ю)=[с(0) - с(*)] ехp(-t,,т), Q)
hегe с(0) and с(эо) сoггеspond to the initial and stablе valuеs, so thе rеlaхation сan bе
rеpгеsеntеd bу a dimеnsionless quantitу as
A(t'Т)т[сt (t)-с (со)]/[сt(0) . с(оo)] = ехp(t,,т1. (3)
Aл exсitеd statе сan Ье сrеatеd Ьy polaгization rд,ith an еlесtгiс fiеld [2 1], bу magnеtiс fiеld
сyсling |22l oг by thеrmal сyсling |2з,9].In еaсh of thеsе сasеs thе геsponsе оf the sуstеm
pгobеs its diffеrеnt pгopегtiеs. Bу srudуing thе tеmpеratuгe dереndеnсе of т, wе сan ехtгaсt
fтom Еq. (i) еnеrgу сharaсtеristiс ofthе transformation, thus еnabling transiеnt spесtгosсopy
of thе respесtive phase tгansitions'
257
Ехpеrimеntal t . ^t ..l I .^l+о ..,orр оhtаinеd as describеd еlsеwhеrе t24] s9чplе
Singlе сrуstars of Сl and l salts wеrе obtainеd as describеd с
sizе was tуpiсallу 1*1*0-1;#;"; сt ,utt
""d
;;;O;-;os I11ч. foг I salt. Standard Dс 4-
Drobr tесhniquе with .',*"i,"r'irn .onau.tlng |йn" *u' used for rssistanсе mеasurеmеnts.
Ьеtailеd t(T) dеpеndе*" *u, mеasurеd on ,*Z Ъ.у'"r' of Cl salt. Annеa'ing еffесt data was
obtainеd on two .u.p.й oi r ,utt anа z sam"pt;;;i аi
'^1'. .Е]::*
for diffеrеnсеs within
unсегtaintу in tье ,еta*uil"li*"l,". bеlow), {ualitativе сoгrеspоndеnсе was obsеrvеd.
Stгuсtuгal rеlaxation studiеs *.," n1uЪТЁ;;;;idR(t) tгansiеnt induсed by thе
thermal суо1е shown in Fig l(a)
6
&,"
140
t20
100
v
(.)
l-r
б
l-r
a.)
-'1
2
40
20
с)
O
{-J(л
(h
()
Fis.l.(a)RеsistanсеtransiеntinClsaltat68KandaГrtofitstailp1:twithaslowехponеnt,
Two vесiсal tin",,ьoJ,tь;;;i;;intе^-at,.in whiсh tеmpеratuт-е.instabi,ity is largеr than
t0.01 K. Timе diagra*.-o? iь" ,h:ч1l "у.ь
u,"d in thе rrsistanсe rеlaхation studу
сoгresponds tо thе гiдt sсatе. чlj::'j.еd
rеsistanс,е transiеnts .4т(')= [rRт(l) _
;;-'r,"й;.й - л,,,.] at s.еvеral rеprеsеntativе tеmpеraturеs.
After еstablishing a standaгd initial.statе'bу annеаling.at l?01^э', hrs, геsulting in thе
stablе and rерroduсiblJ.;;;;";" R(l?.O5) il-...й .йrе, thе samplе was qurпсhеd into
liquid hеlium. Thus a;;;;i;;;;-.quпiь,iu..iniiiut ,'u,. was сrеatеd. and its rеlaхatlon was
stцdiеd bеlow 120 *''i;;?,,;;;;;ii9 K p#;;;tiьn тl. .samulе
was brought to thе
targеt trmpеrature bу Т"o,} *.,Т'"g c к/Ь;)";;;";.; n--This pioоеdure еnablеd rapid
lуp",,i
"
g
.
of t!1' hi gh-t еm pегa."l.
-,1,"9j: "ft :*к:- l;^':;пffi::liliЁ :."'i'':l';1:.;
!;:r*ъ*:Е}:]l"'l-''':Тffif ::il;Н:iтЁ:1'.yy"5.."fi '::iy;.H-':JiH;:T.
еxcееds t0.0lK. Thе";;;;;й"n oг. in this сasе еnсountеrеs sornе pгoblеms, slnсе tnе
most сhaгaсtеrtsttс lnttial paгt of the n*,i.n..i, n"ip,..i'. Kееping this in mind, wе adoptес
thе following,.ь".",lf i,un,i"ш *.:Y::'Ji{lь чis; H"я'iЫ .1,ъ;J ;цliЦ Ц.
*i::i**.;1:::Н}::i:'T li:] :1 }i;:Ёi;": Ё,ёii,i,i'(,l . Дт(.о)l Thе stead.'
I o experimenl
1
-
r, eхponеnt frt
i-
Timе (sес)
258
[2a]. Samplе
лdaгd DC 4-
еasurеmеnts'
iесt data was
'enсеs within
sегvеd.
сuсеd by thе
]. :
-'\' ехponеnt.
' .s largеr than
::.i:ation study
-,= [Rт(l) _
-..rlting in thе
:-эnсhеd into
i .. зхation was
. :-:ught to thе
з .-зblеd rapid
tl:еcrеased т
Ц-
-еsulting in a
в'j :empегatuге
rtе--s. sinсе thе
]г : ''\,е adoptеd
rг ]- aftег first
! ..,nsiеnt was
liс Тhе stеad}'
statе valuе Лт(.) : Л1'55 WaS u.sеd as a fitting рaramеtег to obtain anof thе tгansiеnt tail This *"* айi',*,;;:^:j:-,:,:,""]:l ." {Jolaln an ехроnеntial dеsсription
p ot (Fig l (b)). Тh;' tЦl] ff н цi ii::"ff i;}::x":::"i.?;' ffii tffi:'a'f. ;,;thе геlaхation timе in thе tail iart of thеi?ln,i.nt т: Y1s;;;;;1 *ьit" tь" arnрlitude,4: ofthе сomponеnt was dеtеrminеd г'.o*
"*t.uщration Ъf
'ь.
Ii".". l"i oГ thе рlсlt till сгossingthе l aхis at /:0 Тhеn thе tгansiеnt *u..пit.а bеyond.ь" !"lс.i,-е lntеrval by a two.еxponеntial deсaу funсtion, А1(t) : А{D eхp (-tlт) +.Аz(D ехp (-t/т2),Тt (т;. This proсеduгеallowed us to obtain а satisfaсtory лt at ali j though tь.i. is an un."пuinty оf т2 в,ithin afaсtor of two and геlаtеd smallет un..nui*i", in-thе valuеsЪ *ь.. paгamеtеrs duе toambiguity of thе pгесisе Лtss сhoiсе in stеp 1ij
Rеsults
An Атгhеnius гlоt, of^r9s]stanсе trmpегatuге dеpеndеnсе in Сi salt, mеasuгеd onwaгmlng and сooling at a гatе of l K/min. is shЬwn in Fic-2-
-IУ,
6)
O
-
(л
v1
(.)
Fig.2. Tеmpегatuге dеpеndеnсе of thе геsistanсе of Сl salt measuгеd оn r,''arming and сooling(small сiгсles). Теmpегatuге dеpеndеnсе oГthе initial Л1(0) and steady statе R155 uu'u.,, u,"Jin transiеnt fit (largе оiгсlеs).
Л(| shorvs notablе hysteгеsis, similаг to pгеv,ious герoгts U7 |91 .rhе
hу,stегеsis r,,,asaсtually рrеsеnt at all tеmpеratuгеs studiеd, staпing from roЪm tеmpегaturе, though itsmagnitudе inсrеasеs notablу bеIorv 70 к, almost сoinсiding with thе Arгhеnius plot slopеlnсгеasе It is woгth noting.that warrning aftег quеnсhing*ga"е nеaгly thе samе R(| asobtained on u,aгming aftеr slow сooling,Ъont.ury to в. anаЪ-Bг saits. Figure l(b) showsnoгmalizеd rеsistanсе tгan.siелt in log 7 rs. t jь't ut s"'..ui ,.p.","n.u,iuе tеmpегaturеs.Bеlow appгoхimatеly 50 K thе plot Гs linеaг foг almost thе full intегva] studiеd, At higheгtеmpегaturеs notaЬlе non.linеaritv is obsегvеd in thе initiaiЪui,'inсi.uting thе еssепtial
1llul
l
l
I
l..Г_4q. '0 il(! зo * 2О,"]
dtr*Б;-l
l
_-_ -
---..--_, ]
] . R.(Т) rvaгmlng i ]
j.) У
сontгibution of thе гapid "t1 L:оlТlpoПеltt'
.[hе valuеs оf Л1(0) and Лт,ss usеd in thе transiеnt
linеarization arе shown in ijig,2 1.hеу сoinсidе Iеasonablу with R valuеs measuгеd on
warming and сooling, indiсating а laсk оf long-tеrm R(| сhangе to.'vards a nеw statе'
сontгary to that found in tsr and D-Bг salts [9-l5]
This оonсlusion ц'as additionallу сhесkеd bу lоng tегm annеaling (100 hrs) in thе
viсinity of thе sесond ordег tгansition, Annеaling was pеrformеd at tеmpегatuгеs in thе
intегval 7з + 10 K foг Сl salt and 84t l0 K for I salt with a stеp of l K. Wе havе not found
anу deviatiоn cгЛ(i) bеуond the hуsteгеsis сuгves for both salts, suppoгting thus the laсk of
the long-tеrm tгansformation intо any new statе'
In oгdег to undегstand this striking diffегеnсе bеtwееn Сl and Br salts we shoц' in
Fig'3 thе tеmpеratuгe dеpеndenсе of геlaхation timе for slow and гapid сomponеnts, тl(Т) and
тz(T)
r(K)
lО0
"88 а. i. !ооо8 о
vv v Сlт,
A С|т,
a D-Br
oBr
20 30,
1000/z (K-')
50 2О
i0
O
a.)(л
Р
А
IU:
t0i
10
504010
Fig.3. Tеmpеratuге dеpеndеnсе oГ thе геlaхation timе foг thе rapid (т1) and slow (т2)
сomponеnts of thе trаnsiеnt in Cl sa[t, shown in comparison with т Гoг Br and D-Br salts [8].
Foг сomparison в'е show т(T) in Bг and D.Br salts [9] As сan bе sееn, nеithеr thе гapid nоr
slow сomponent of thе transiеnt in С1 salt show notablе dеviation bеуond an ехpегimеntal
sсatteгing upon passing 13 K sеcond oгdеr phasе transition. on thе othег hand, thе
tempегaturе dеpеndеnсе of thе amplitudе of thе гaрid сomponеnt А1 {.Jig,a) shows notablе
suppression bеlow appгoximatеly 50 K, sо that thе rеlaхatiоn bесomеs nеarlу ехponеntial
bеlow this tеmpеIatulе.
Fig.5
сirсlеs
алd l
еr'аluа
guioеs
supеrs1
phаsе
.l,еrtlса]
providе
/.ov
100
]е tгansirnt
е]surrd on
nе\,v statе,
hгs) in thе
-геs in thе
е not found
. :hе laсk оf
^ е show ln
:s. тr(T) and
s.low (т2)
salts [8].
r-:гaрidnor
в ...рerimеntal
ш:- hand, thе
i'. .'i.s notablе
п" зхponеntial
( i{)-,ЗО 1z-
1.0
О
O()a
P
2000
I 500
1 000
s00
0
f*ы О5\
dеad timе
a
Т..
LY
c
2О
ta}a I T
Fig'4. Tеmpеraпше depеndеnсе оf ihе : ;lnd
сomponсnt is zеrо rуithin ехpегimсntа1 sсаllс:jnq
] Bеi'.rrl. liрproхtirrаteir' .50 K thе amplitudе of tho гаpid
|2О
SS
^^, -^ /"" ./
a
SS
O-"'SS+OD
OD+55Y "lt,
I Cl lD-Br Br
-1 0 l
Рrеssurе (kbaгl
Fig.S. Phаsе diagrаm of thе 80 K tталsitiоn opеn сirсlеs slroп iосаtiоп оf ilrе lrr'stеrеsis braлсhеs [8], solid
сirсlеs coггеsрnd to tlrе sесond oгdtr phаsе tгaлsitiоп [l7-l9.9] Dashеd аrеa shorl'i шaлsГoпnаtiоn
"а,,gЪ
in сt
алd I salts. Cl sаlt is used as a rеfеrеnсс for prеssuте sсаiс Роsttiопs оf D-Br алd Bг sаlts oп ilrе sсаlе аre
еl,aluated from соmparison оГехpегimеntаl Р.Т dlаgгапls [2-5-2j]. posir'rоn of l r.rlt ls аrbitrtuу-. Shоп фshеs arеguioеs foг е}.es fоr thе uppеr and ]orrеr h-r,stеrеsts brarсIlеs Sоiid linе сопеspoпds to thе sесond ordеr
supегstгuсturе -юrdеrеd phаse (SS-oD) tгaлsition, long dаshеs сoпсsроnd to а ПnЪ of the supегstruсtrге sй.pМsе (SS.SS') sесond отdег tгaлsition' N{еtal.tnsulаtоr рrеssure boundаrr,is shоrl,n liith а dashеd{ottеd
r,еrtiсal linе. The sub-phаsе bоundап,сan bе tгассd in1о tlrе ordеrеd phаsе aлd саn bе obsегv.еd ехpегimentаlly,
providеd t-Iiе trалsfoгmаlon is rnсomolеtе
a
0.030, 40
(K',)
50
\./
P90
Ф
ь.Jr А^
с)
ta
Lr-
261
Disсussion
WеsummaгizеdthеeхistingdataaЬout80Ktransfoгmationinthеpressuгr.
tеmpeгatuге (P-T) phasе diagгam Gi;:) .To еstablish prеssurе sсalе wе usеd ехpеrimеntal
аi;й;;' foгtCl and в.
'uit'Tз,s,
zЬ-il1,'shоwing that thе diagгams for Сl' D-Br and Bг salts
сan bе matсhеd bу a shift in pressurе, apрroхimatеlу 0.3.0.4 kЪaг pеr salt [25-27], Thе
p"'i'i"" oi i surt on thls diagram is not сlеai. Inсrеasеd stabilitу of the insulating statе in thе
!.r,
'"
prеssuге [1,3] сan iidiсatе a fuгthеr shift into thе insu1ating statе from thе metal-
insulatoг boundaгy. on the othег hand, from сonsideration of thе lattiсе сonstants it сan bе
arguеd that thе salt оorrеsponds to highег рrеssurе [4] and maу bеlong to a nеw insulating
domain [2s] Wе
"un
u..ung. thе salls in.thе sеquёnсе Cl - Ч-B'-- Br, сoггеsponding tо
inсгеasing pгеssurе, unс pTo' thе data .fгom thЪгmal ехpansion Il7-19] and rеlaxation
mеasurеmеnts in thе..1"iйЬгше mеtal-insulator prеssure ь9}lduy as shоwn in Fig 5. Thе
dashеd arеa foг Cl salt геpiеsеnts thе tеmpегaturе rangе in whiсh thе amplitudе of thе rapid
сomponеnt is not еqual to zеro.
Тhе геsults of this studу show еssеntial diffеrеnсе in thе 80 K transformation
bеtwееn thе salts. Тhis diffегеnсе bесomes moге еvident whеn analyzing thе phasе.diagram
As сan bе sееn fгom Fig 3, thе width of thе intегval of the ordегing trаnsformatiоn, involving
сrossing of thе 2000 к Бйiе., sharplу dесreasеs from Bг to D-Bг salt, mainlу duе to thе гapid
deсrеasе ofthе tеmpегaturе ofthе uppеr hystеrеsis branсh. Ехtгapolation towards thе prеssuге
boundary impliеs .,o,,й! of thе branсhеi so the absеnое of this rangе in Cl salt sееms to bе
systеmatiс' This сonсlusiБn finds support in.thе ехisting data foг Cl salt undеr prеssurе. In thе
viоinitу of pгеssurе b";;;ы ;; i s j Ёar геsistanсе геlaiation bесomes qualitativеlу similaг to
BгandD-Bгsalts[29].Thus,thеsamеtransГoгmation,thoughtakingplaсеЪothinthе
mеtalliс and insulatin*-,]ь"'.i i' notuьty diffеrеnt on both sidеs of prеssurе boundaгу, namеlу
in thе laсk of 2000 K transformation rangе.
on the ott,., Гu"J, tь" rеlaxatйn phеnomеna bеlow thе lоw tеmpеratuге hуstеrеsis
branсh aге similaг Gi;.;j'-;h"*iй сегt;in similarity of thе respесtivе statеs...SiT']il
сoпеsponden""
"*ist,
ьБt*"еn rеlaxa-tion phenomеna iniuсеd bу magnеtiс fiеld cусling [22l
in thе both salts.
Thе linе of seсond оrdеr phasе transition sееms to havе a minimum in thе viсinitу оf
the boundary prеssuIе |25-271. Тhis сonсlusion сan be madе bу traсing assoсiatеd anomalу in
rеsistanсе tеmpеraturе dереndеnсе undeг prеssure, usеd to plot prеssurе diagrams for Cl and
D-Bг salts. It сan еvеn bе сonsidеrеd as two
".o*,ing
linеs сoming with diffеrеnt inсlination
fтom the insulating (с1) and mеtalliс (D.Bг and Bф iomains (in viеw of this faсt and highег
tеmpеratureofthe sесond ordегtransition' wе plaсe tеntativеlу I salt to the lеft of thе Cl salt)
Howеvег, сommon to ьotь mеtalliс and insuiating domains, bеsidеs thе transition itsеlf, is
obsеrvation of a.halo' of rеlaхation in its viсinity
WеstaгtthedisсussionwithBrsalt'inwhiсhthе80K.tгansГormationisdеsсribеd
wеllbуapsеudo-spi"".п.ьl.modеlofеthуlеnеordегing(Ео)t3O]ordегingofеthуlеnе
gгoups on соoling p,o...с, in two stagеs: (tj frееzing of Бthуlеnе motion (at 160 to 200 K)
lеads to an inсomplеtе оrdеr (supегstruсtu,. phu,., s5); tzl tiansfoгmation to thе сomplеtеlу
oгdегеd phasе oD p,o.".а, on п,,tь., оooliф- ьу '..*а
o'а.'^Phase tгansition at 80 K' Thе
transformation (2) aсtuallу proсееds in a broad tеmреratuге rangе in thе viсinitу of SS to oD
phasе transition (indiсatеi in thе еxpегimеnt ьу тiт) anomaliеs,,.Fig.3). This pесuliarity is
сaused by thе p'.,"n"Joi.*o miniйa of frееЬ"';i with a s-ma1l епегgy diffегеnсe (of thе
ordеr oftempеraturе), sеparatеd by a high potеntial ЬЬr.ie.; and smooth сhangе ofthis enегg}'
differenсе on сooling. This lеads tо laгgе mеtastabilitу effесts [3 1] Ехistеnсе оf SS abovе 8О
K was indееd foцnd in ,.u.,ut studies (+,s,зz1in вr salt. The сoехistеnсе of two phasеs in thе
transfoгmation l.ung.-*u, obsеrvеd in-thе ЕdR speсtгa of quепсhеd samplеs [33] Howеvег.
соmplеtе ordеring p,.Jй.а ьy the modеl гoiш. statе belоw 60 K, although сorrеsponding tо
:o'
:. thе prеssuгe-
*.J ехperimеntal
)-3r and Bг salts
z.: 125-271. The
::::g statе in the
:эm thе mеtal.
:.:]nts it сan bе
: зеw insulating
::::еsponding to
.rd rеlaxation
.': :n Fig.S. Thе
:.-з ofthе rapid
r':-аnsfoгmation
r .1]sе diagram.
:.' ':r, involving
i ] -:. to thе гapid
ьr::s lhе prеssurе
: :: : seems to bе
r :-:ssurе. In thе
Еt: ..''' similar to
ш:.. :oth in thе
ш: -. ]aгу, namеly
E*: --3 hysteгеsls
: r:is. Similar
ffie : :lсling [22]
thе геsults оf stпtсtuге dеtеrmination [7], is in сonfliсt with thе ехistепсе of SS at lowtеmpегatuгеs in high геsоlution Х-ray data [5] and thе nоtablе anomaly in геlaхatiоn tirnеtеmpегatuге dеpеndеnсе [9] . Тhis disсrеpanсy sееms to aгisе fгom intеraсtion bеtwееnсonfoгmational ordeгingand thе.еIесtтoniс systеm [9'3з], not сonsidегed in Еo modеl [3O]For thе appliсatiоn of thе Еo modеl tо С1 and i salts, wе have to assumе thе laсk ofсоmplеtе oгdег upоn thе frееzing of еthуlеnе motion at aгound 200 K [34] and thе foгmationoГa supеrstruсturе in a sесond oгdег tгansition^t.зо] In I salt .*;,,ing еxpегiments suppoгt thismodеl. Sесono огdег tгansitiоn is оbsегvеa at zзo k [18], and tui!".аi,o.a"r at tzi * .'i;;"bе assignеd to thе unгеsolvеd SS oгdег, Мoге difftсuitlеs arisе-*hеn dеaling with Cl salt'Dеspitе oГ notaЬlе anоmalies in thе thегmal ехpansiоn' u
'..ona ordеr tгansition \'!,as notdеtесtеd. siп-rilaг tо Bг salt [17] Fоггпation of thЪ SS at aгound 1бO K was геpопеd oпly inFТIR and Raman studiеs, dirесtly pгoЬing thе еthуlеnе f?.;;";;Ъг,ь. molесulе and thесlosеlу rеlatеc CN bond in thе pоlу mе.rс aiion Jо1 iг tьis intJ.p."iution is сoггeсt'
"i""g
йьsmall thегmal faсtогsоfсaгbonatomsat 127KinАthеlaсkoгjеtесiaьtеSSгеflеctionsinthе
Х.гaу [5i, it may indiсatе small amplitudе оГmodulation of thе..ii|'"с сonformation in thс.эгуst al '
Stаbilizatiоn oi йе SS statе upon plеssurе dесrеasе, as pгеdiсtеd bу the Еo modеl
[30]. соuli ехplain thе diffегеnсе in thе геlaхation phеnomеnu ь.'*..n Сl (and I) and Br (andI-l-Bг) salts' Horl'еvеr' aссоrding tо thе modеl, thе SS-OD boundaгy should go to zеrotеmpегetuге on prеssurе сiесгсаsе and no sесоnd oгdег tгansitiоn shoLr]c bе obsейеd withinthе. SS phasе z\t this point it is vi,oгth,,vhilе to rесal1 thе disсгeрanсy bеtweеn tье е*pе.lmеntand thе rnodе] fоr Br salt [9,33] at thе lоw tеmpеIatuге tгansfoгmation boundary and thеsrmilaгitv of thе геiaхation foг Сl and Br salts bЬlor^., this line (гig з;. In viеw of notableсhangе оi еlесtг..lniс рroрегtiеs at this bounсiaгy it is natural to
.сo"nсludе
a сontгibution ofе]есtroniс еnег.s}'into thе tгansfoгmatiсln. All thе prеdiсtеd fеaturеs oГthе Еo tгansfoгmatiorrhojd ila sub-phаsе tгansГormatiоn (SS to SS') оf thе supеrstгuсtuге-takеs plaсе instеad of atгansfoгпration into an oгdегed phasе, pгovidеd thе SS' is morе stablе than the oо pьas" Ъiеr,еn thе smallеst е]есtгoniс еneгgу gain If thе еiесtгoniс enегgy еffrсts thе pгoсеss, foг itsdесrеasе thе sub.phasе tlansformation should рush thе еlесtгйiс systеm of thе сompoundtоwaгds arr insulating statе' Тhis is indееd sееn in R(Т) in Сl saй as an inсгеasе of thеасtlvatlon еnегgy in the tеmpегaturе гangе of thе traлsformation (Fig.2)' An еlесtгoniс еnегgуgain should beсomе moге impoпant upon prеssuге dесгеasе, ,inсЪ 1T; a рuгely struсtuгal gainin thе oD phasе соmpaгеd to thе SS рhasе dесrеasеs, and (2) un .t..t.oni. .n..gу iulninсrеasеs duе to an inсгеasе in thе dеnsiiy of statеs. Thегefoге, ii is natuгat to ехpесt a sub-phasе tгansfогmatiоn at highег tеmpеraturе with pгеssuге dесrеasе, as is indеed obseгvеd inthe insulating phasе Similarly to the ordегing trinsformation' thе sub-phasе tгansfoгmation
should pгoсееd thгough сoехis-tеnсе of two phasеs in somе tеmрегaturе гangе, giving thесhaгaсtеristiс transfoгmation .halo' Тhus thе nеt еffeсt of thе tгansfbrmaйon-is siгеad
thгough thе 100 tо 5О K rangе, whiсh сould ехplain thе iaсk ofshaгp сhangеs in еlесiгoniсpropегtiеs In addition, in Iinе w,ith thе data оf Ёig з, thе сhагaсtегistiс еnещу of SS to SS,
tгansfoгmation should bе еssentialiу rеduсеd сompaгеd to that of Ss to oD, siйсе only a small
numbег oГthе molесulеs сhangе thеiг сonfoгmational state'
In viеw of this, it sееms геasоnab1е to intегрrеt thе 80 K transfoгmation in Сl (and I)
salt as a sub.phasе tгansitiоn in thе superstruсtuге phasе, и,hilе in mеtalliс Bг and о-вг salts
thе tгansfoгmatiоn hеads towaгds an oгdегеd statе. Тhis intегргеtation supposеs that in Br saltss-oD lransloгmation takеs plaсе at a highеr tеmpеratuге than thе sub.phasе transfoгmation.
Тhе lattег сan still bе obsегvеd in a mеtalliс statе if еithеr oгdегing tгansformation isinсomplеtе, oгthе SS'phasе bесоmеs moге stablе than thе oD on fuгtheг*сooling In cr 1uJI) salts sub-рhasе tгansfoгmation takеs plaсe at a highег tempегatuге than tйe o.dе.ing,
геsulting in a stab]е stlpегstruсtuге phasе at lоrv rеmреraturеs.
. i'iсinitу of
:nomalу in
. Ъr Cl and
.lnсlination
- зnd highеr
':.е Сl salt).
:. itsеlf, is
. Jеsсribеd
: еthylеnе
:o 200 K)
':'rrplеtеlу
:] K. Thе
,SStOOD
.:-,iaгity is
. .е (of thе
.ls еnегgу
. :bovе 80
:.эs in thе
rcwevег'
rding to
Cоnсlusion
Seсond oгdег phasе tгansition obsеrvеd at aгоund 80 K in thе family of oгganiс
supеrсonduоtors к-(BЕDТ-TТF)zCu[N(сN)2]Х is aссompaniеd by notable diffеrrnсе in
lattiсе геlaхation and thе annеaling effесt, dеpеnding on whеthег it is an insulating (Cl and I)
oг a supеrсonduсting (Bг and D-Br) salt. Wе гelatе this diffегеnсе to thе differеnсe of еthуlеnе
oгdегing in thе ground statе as a геsuit oГ сompеtition bеtwеen sub-phase and oгdегing
tгansfoгmations of thе suDеrstruсturе ohasе.
Aсknowlеdgement
Тhis work has bееn suppогtеd by CRЕSТ from Japan Sciеnсе and Тесhnology
Сoгporation and bу Kyoto Univегsitу Vеntuге Business laboгatory' М A.T aсknowlеdgеs
suppoгt from Japan Sосiеtу foг thе Ргomotion of Sсiеnсе.
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jiffегеnсе in
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е ofеthylenе
and ordеring
l Тесhnologу
lсknowlеdgеs
t \1,Kini, аnd
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, -- 58, k2944
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| id | oai:ojs.pkp.sfu.ca:article-65 |
| institution | Surface |
| keywords_txt_mv | keywords |
| language | English |
| last_indexed | 2025-09-24T17:44:40Z |
| publishDate | 2001 |
| publisher | Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine |
| record_format | ojs |
| resource_txt_mv | surfacezbircomua/f7/ba934ef6be8202f47e7fe52937e6c4f7.pdf |
| spelling | oai:ojs.pkp.sfu.ca:article-652018-11-27T09:42:39Z Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) Tanatar, M. A. Ishiguro, T. Kushch, N. D. Yagubskii, E. B. Second order phase transition, observed previously in the title salts in thermal expansion studies close to 80 K, was studied in insulating X= Cl and I salts by a transient spectroscopy of structural relaxation and by controlled annealing. A notable difference in the activation energy of transformation and in annealing behavior compared to the metallic X= Br salt was found, showing transformation towards different structural states at low temperature. &nbsp; Second order phase transition, observed previously in the title salts in thermal expansion studies close to 80 K, was studied in insulating X= Cl and I salts by a transient spectroscopy of structural relaxation and by controlled annealing. A notable difference in the activation energy of transformation and in annealing behavior compared to the metallic X= Br salt was found, showing transformation towards different structural states at low temperature. &nbsp; Second order phase transition, observed previously in the title salts in thermal expansion studies close to 80 K, was studied in insulating X= Cl and I salts by a transient spectroscopy of structural relaxation and by controlled annealing. A notable difference in the activation energy of transformation and in annealing behavior compared to the metallic X= Br salt was found, showing transformation towards different structural states at low temperature. &nbsp; Chuiko Institute of Surface Chemistry National Academy of Sciences of Ukraine 2001-06-10 Article Article application/pdf https://surfacezbir.com.ua/index.php/surface/article/view/65 Surface; No. 4-6 (2001): Chemistry, Physics and Technology of Surface; 256-265 Поверхность; № 4-6 (2001): Химия, физика и технология поверхности; 256-265 Поверхня; № 4-6 (2001): Хімія, фізика та технологія поверхні; 256-265 3154-8091 3154-8083 en https://surfacezbir.com.ua/index.php/surface/article/view/65/64 Авторське право (c) 2001 M.A. Tanatar, T. Ishiguro, N.D. Kushch, and E.B. Yagubskii |
| spellingShingle | Tanatar, M. A. Ishiguro, T. Kushch, N. D. Yagubskii, E. B. Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_alt | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_full | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_fullStr | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_full_unstemmed | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_short | Transient spectroscopy of 80K second order phase transition in k-(BEDT-TTF)2Cu[N(CN)2]X (X= Cl, I, and Br) |
| title_sort | transient spectroscopy of 80k second order phase transition in k-(bedt-ttf)2cu[n(cn)2]x (x= cl, i, and br) |
| url | https://surfacezbir.com.ua/index.php/surface/article/view/65 |
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