6G asas y Acei es
Vol. 51. Fasc. 1-2 (2000), 6-25
RESUMEN
Compo amien o eológico y de ase de lípidos an i ílicos
En es e capí ulo se ealiza una e isión de las dis in as
es uc u as coloidales de asociación que pueden o ma los
lípidos an i ílicos en es ado líquido-c is alino y de sus
co espondien es p opiedades de lujo en cizalla. Se desc ibe la
es uc u a y compo amien o eológico de c is ales líquidos
e mo ópicos, con én asis en los de ipo esméc ico, ases gel, y
c is ales líquidos lio ópicos: nemá icos, lamina es, lamina es
diluidos, dispe siones de lamina es, hexagonales y cúbicos. Se
hace hincapié en la impo ancia de una buena ca ac e ización
eológica y eo-óp ica de ca a a sus aplicaciones p ác icas,
desa ollo de o mulaciones y como una écnica ú il pa a
de e mina diag amas de ases y de ec a cambios de es uc u a.
Se ha usado una me odología his ó ica pa a analiza la
e olución de la ca ac e ización eológica e iden i icación de las
di e en es es uc u as líquido-c is alinas y es uc u as a ines. La
in e p e ación de compo amien os de lujo iscoso no
new onianos, enómenos ixo ópicos y an i ixo ópicos y de las
p opiedades iscoelás icas lineales, de e minadas con ensayos
dinámicos y de luencia, y no lineales, desc i as median e la
di e encia de es ue zos no males y ensayos de elajación del
es ue zo, se basa en la in e elación mic oes uc u a-
compo amien o eológico. La na u aleza polic is alina de los
c is ales líquidos esul a se muy sensible a la cizalla, debido al
cambio de amaño y o ien ación de los dominios líquido-
c is alinos mien as luyen.
PALABRAS-CLAVE: Compo amien o de ase  Compo a-
mien o eológico  Lípidos an i ílicos.
SUMMARY
Rheological and phase beha iou o amphiphilic lipids
This chap e e iews he di e en associa ion s uc u es
which a e likely o be o med by amphiphilic lipids in he
liquid-c ys alline s a e and hei co esponding shea low
p ope ies. The s uc u e and heological beha iou o
he mo opic liquid c ys als, emphasizing he p ope ies o smec ic
mesophases, and hose o lyo opic liquid c ys als such as:
nema ic, lamella , dilu ed lamella , lamella dispe sions, hexagonal
and cubic mesophases a e desc ibed. The impo ance o a
comp ehensi e heological cha ac e isa ion, including heo-op ical
echniques, is poin ed ou o hei p ac ical applica ions,
de elopmen o o mula ions and as a use ul echnique o assis in
he de e mina ion o phase diag ams. A his o ical app oach has
been used o discuss he e ol ing ield o he heology and
s uc u e iden i ica ion o liquid c ys als o med by amphiphilic
lipids and su ac an s. Non-New onian iscous shea low,
hixo opic and an i hixo opic phenomena, linea iscoelas ic
p ope ies -desc ibed by dynamic and c eep compliance
expe imen s- and non-linea iscoelas ic p ope ies - desc ibed by
he di e ence o no mal s esses and s ess elaxa ion es s a e
in e p e ed on he basis o a mic os uc u e- heology ela ionship.
The polyc ys alline na u e o liquid c ys als u ns ou o be a he
sensi i e o shea due o he change o bo h size and o ien a ion o
he liquid-c ys alline monodomains unde low.
KEY-WORDS: Amphiphilic lipids  Phase beha iou 
Rheological beha iou .
INTRODUCTION
Amphiphilic lipids con ain a hyd ophilic head and
one o wo hyd oca bon long ails in he same molecule.
The o me ends o dissol e in wa e o pola
sol en s, while he la e ends o do so in nonpola
sol en s. As a consequence, hey o m associa ion
s uc u es, abo e bo h a c i ical empe a u e and
concen a ion, in o de o educe he ee ene gy in
he sys em o a minimum.
Depending on he chemical na u e o he
amphiphilic lipid, wa e concen a ion, empe a u e,
and he concen a ion o addi i es such as di e en
oils, ino ganic sal s, alcohols and suga , di e en
ypes o associa ion s uc u es (micelles, lyo opic
liquid c ys als -also called lyo opic mesophases-,
gel phases) can exis in hese sys ems. Such a
ascina ing a ie y o associa ion s uc u es leads o
he occu ence o a wide ange o heological
p ope ies (Muñoz e al, 1989, 1991). In u n, his
means ha a ailo -made heological esponse o an
amphiphilic lipid sys em can be achie ed by
calcula ed changes in mic os uc u e (Ba nes,
1980). Con e sely, heology may assis in he
de e mina ion o phase diag ams since i is
sensi i e no only o changes o associa ion
s uc u es bu also o a ia ions o bo h composi ion
and empe a u e wi hin he ealm o exis ence o a
pa icula phase o mesophase (Rounds, 1994),
(Dimi o a e al, 1995), (K öge , 1996). This is due
o he ac ha he heology o amphiphilic lipid
sys ems is dependen on he physico-chemical
in e ac ions go e ning he associa ion s uc u e
o med.
Rheological and phase beha iou o amphiphilic lipids
By J. Muñoz and M.C. Al a o
Depa amen o de Ingenie ía Química,Uni e sidad de Se illa. Fac. de Química
C/P. Ga cía González s/n. 41012-Se illa (Spain)
[email p o ec ed]
E en hough some p og ess has been made in
he heo e ical calcula ion o phase diag ams
(E ans and Wenne s öm, 1994), i canno be
denied ha he ac ual de e mina ion o phase
diag ams elies on expe imen al wo k. In ac , he
inc easing use o new o imp o ed echniques has
e ealed signi ican e o s in ea lie phase
diag ams, mainly s udied by isople hal ins ead o
iso he mal me hods (Laughlin, 1990). Besides
classical echniques such as di ec obse a ion,
cen i uga ion, pola ising mic oscopy ex u es,
dila ome y, calo ime y and small-angle x- ay
di ac ion, Laughlin (1990) ci ed deu e ium (o
phospho us) nuclea magne ic esonance,
imp o emen s in calo ime ic me hods and he
«lyo ope g adien » p inciple, as ecen echniques
inc easingly used o ca ying ou phase s udies.
Addi ionally, elec on mic oscopy echniques,
such as eeze- ac u e elec on mic oscopy o
c yo- ansmission elec on mic oscopy, small-angle
neu on sca e ing, ligh sca e ing, ime- esol ed
luo escence quenching along wi h e ined
heological and heo-op ical echniques mus also
be aken in o accoun .
A u he ype o associa ion s uc u es o med
by amphiphilic lipids a e he mo opic liquid c ys als
(also e e ed o as he mo opic mesophases),
which a e o med a empe a u es emb aced
be ween hose co esponding o he pu e c ys alline
s a e and he ac ual mel ing poin o he amphiphilic
lipid. In his chap e , all he ypes o he mo opic
mesophase s uc u es will be co e ed o he sake
o comple eness, e en hough amphiphilic lipids
basically o m smec ic mesophases.
Liquid c ys als ha e in e es ing applica ions in
di e en ields: in he de e gen and ela ed
indus ies (Ba nes, 1980), in he cosme ics indus y
(Comelles e al, 1994), in pha macy, as ehicle o
solubiliza ion media o ac i e p inciples, in biology,
o memb ane simula ion, esicles, ex ac ion o
pep ides and p o eins (Golds ein and Leible , 1987),
(B own and Wolken, 1979), in he ood indus y (K og
e al, 1985), (Söde be g and Ljusbe g-Wah en,
1990), (La sson and Dejmek, 1990), (Kim and
Baianu, 1991) in emulsion echnology, as s abilise s
since hey may impa sui able heological
p ope ies o he d ople in e ace and o he
con inuous phase (Pilpel and Rabbani, 1987),
(Riego and Gómez He e a, 1988) and so on.
Micelles will no be add essed in his e iew
since hey would equi e a ull chap e o hemsel es.
This wo k ocuses on gel phases and on he
di e en lyo opic liquid-c ys alline s uc u es o -
med by syn he ic as well as biological amphiphiles,
wi h emphasis on hei heology.
A his o ical app oach is used o discuss he
con inually e ol ing ield o he heology o
amphiphilic lipids. Reade s who a e no amilia wi h
heological echniques a e e e ed o some
excellen books, such as he in oduc o y-le el
olume by Ba nes e al (1989), he mo e ad anced
books by Fe guson and Kemblowski (1991) and
Macosko (1994) o he undamen al wo k by Fe y
(1980).
CRYSTALLINE STATE
In he solid s a e amphiphilic lipids o m
c ys alline s uc u es which a e cu en ly s udied by
X- ay di ac ion. Thei molecules a e packed in
bilaye s wi h he pola heads loca ed on he ex e nal
plane and wi h he hyd oca bon chains showing a
pa allel a angemen inside he bilaye s. In ac ,
hei packing p ope ies a e simila o hose o a y
acid c ys als.
Lipid molecules show polymo phic beha iou
inso a as hey exhibi di e en packing in he solid
s a e wi h ageing ime and p esen mul iple mel ing
phenomena. Polymo phism is associa ed wi h
changes in he il o he molecules in he bilaye s
and possible o a ia ions in hyd oca bon chain
packing (La sson, 1994).
LIQUID CRYSTALS AND THERMOTROPIC
LIQUID CRYSTALS
Liquid C ys als
Liquid c ys als, also called mesophases, may be
conside ed as an in e media e s a e o ma e
be ween liquids and solids. While in he c ys alline
s a e he mo emen o molecules is p ac ically
es ic ed, liquids exhibi s uc u es wi h sho - ange
o de and molecules can eadily low. Molecules in
liquid c ys als achie e some eedom o ela i e
mo emen while s ill e aining a kind o long- ange
o de . This esul s in s uc u es in which molecules
a e equen ly associa ed wi h a pa allel o
nea -pa allel a angemen .
Liquid c ys als o igina e when a c ys al is
subjec ed o in luences which loosen he hold o he
molecules on one ano he due o ei he a ise o
empe a u e in some cases o he addi ion o a sol en
in o he s. The o me mechanism leads o
he mo opic liquid c ys als and he la e o lyo opic
liquid c ys als, bo h o hem exhibi ing polymo phism.
The mo opic Liquid C ys als
The mo opic liquid c ys als occu when some
pu e o ganic solids o mix u es o solids a e hea ed
and do no pass di ec ly om he solid s a e o he
liquid s a e bu hey o m a semi- luid phase ha
Vol. 51. Fasc. 1-2 (2000) 7
sha es some p ope ies ypical o solids and some
o he s commonly ound in liquids. O dina y
he mo opic liquid c ys als a e usually classi ied as
nema ic, choles e ic and smec ic (B own and
Wolken, 1979). Addi ionally, a la ge numbe o
polymo phic ansi ions can be de ec ed wi h pu e
amphiphilic lipids be ween he c ys alline and he
liquid s a es (Winso , 1974).
Nema ic Liquid C ys als (N)
Nema ic liquid c ys als consis o an a angemen
o pa allel o nea ly pa allel elonga ed molecules,
which a e mobile in h ee di ec ions ( hey do no
o m laye s), due o he lack o a pe iodic
a angemen , and can o a e abou one axis.
Howe e , he mean dis ance be ween molecules is
smalle han hei diame e , hus esul ing in he
o a ion no being ee and in signi ican
in e molecula in e ac ions. This may gi e ise o
complex low p ope ies, al hough nema ic liquid
c ys als exhibi luid-like p ope ies and less iscosi y
han smec ic liquid c ys als. In ac , nema ic liquid
c ys als posses he lowes s uc u al o de in
he mo opic liquid c ys als and hey a e ans o med
on hea ing o he iso opic liquid wi hou undegoing a
u he mesophase ansi ion. They a e uniaxial om
an op ical poin o iew wi h he op ic axis pa allel o
he mean di ec ion o he long molecula axes, he
so-called nema ic di ec o . Howe e , hey exhibi
dis inc i e ex u es-mainly h eadlike disclina ion
lines associa ed wi h s uc u al discon inui ies in he
ma e ial (Ha shone, 1974) when obse ed unde
pola ising mic oscopy.
Choles e ic Liquid C ys als (N*)
Choles e ic liquid c ys als a e some ime classi ied
as a special ype o nema ic liquid c ys als. As he
name indica es, hey we e i s de ec ed wi h
choles e yl es e s. The s uc u e can be desc ibed as
ha o a nema ic mesophase wis ed abou an axis
pe pendicula o he long axes o he molecules.
While on a local scale he nema ic and choles e ic
s uc u es a e alike, on a la ge scale he choles e ic
di ec o ollows a helical o m. As a consequence o
i s s uc u e, his mesophase exhibi s a e y s ong
op ical ac i i y. In gene al, he lack o long- ange
asla ional o de is esponsible o hei luid-like
p ope ies. Howe e , he occu ence o highly
iscous choles e ic liquid c ys als wi h gel-like
p ope ies was epo ed o exis in choles e yl
nonanoa e. These liquid c ys als we e also obse ed
in hose homologues which o m s ongly wis ed
choles e ic mesophases when upon cooling an
iso opic liquid, an iso opic ex u e was i s
obse ed, be o e a bi e ingen ex u e appea ed.
This beha iou was asc ibed o he o ma ion o a
egula la ice o alignmen singula i ies (Saupe,
1974).
Smec ic Liquid C ys als
In smec ic liquid c ys als he elonga ed
molecules a e essen ially pa allel o one ano he ,
and a e a anged in laye s wi h he mean di ec ion
o he long axes o he molecules no mal o he
laye s. This e m is de i ed om he G eek
«smec os», whose meaning is «like soap», and is
used because alkyl ca boxyla es o m mesophases
o his ype.
Smec ic liquid c ys als a e luid bu a mo e
iscous han nema ic liquid c ys als. Thei luidi y is
due o he lexibili y o he laye s and also o he ac
ha in e laye a ac ions a e weak compa ed wi h
he la e al in e molecula o ces and, he e o e he
laye s can slide o e each o he qui e easily while
s ill emaining essen ially pa allel. Fo his eason,
hey can exhibi di e en cha ac e is ic ex u es
when obse ed unde pola ising mic oscopy, such
as homeo opic, ocal conic, «bâ onne s» and an
like ex u es. Smec ic liquid c ys als may be
classi ied as s uc u ed o uns uc u ed phases
depending on he molecula o de wi hin a laye . A
comp ehensi e s udy o polymo phism o his kind
o liquid c ys als was gi en by Demus e al (1983).
Idziak e al, (1994) used a Coue e shea cell
wi h concen ic cylinde s which a e anspa en o
x- ays o de e mine he o ien a ion o a smec ic-A
liquid c ys al as a unc ion o he shea a e. A low
shea a es he o ien a ion was no uni o m bu a
he e ogeneously mixed polydomain ex u e wi h
laye s andomly o ien ed pa allel o no mal o he
low di ec ion. A high shea a es, a homogeneous
o ien a ion egime was obse ed whe e he laye s
o ien ed pe pendicula , by no means pa allel as
could be expec ed, o he low di ec ion.
The occu ence o he mo opic mesophases in
amphiphilic lipids is a consequence o a balance o
he s ong a ac ion be ween hyd ophilic head
g oups and he weak a ac i e o ces be ween
hyd oca bon chains. Soaps a e among he mos
well-known amphiphilic lipids ha o m he mo opic
liquid c ys als. Di e en s uc u es (mainly ibbon,
disc and lamella phases) ha e been p oposed o
exis in hese sys ems (Winso , 1974), (Tiddy,
1980). Tamamushi (1974) epo ed ha smec ic
liquid c ys als, like he co esponding lyo opic
lamella mesophase, o med by ammonium
sal s o highe no mal ca boxylic acids exhibi ed
non-New onian (pseudoplas ic) heological p ope ies
a in e media e shea a es and maximum alues o
appa en iscosi y a he mel ing poin o he liquid
c ys al. A u he compa ison be ween he heology
8G asas y Acei es
o he mo opic and lyo opic liquid c ys als can be
made wi h he e na y sys em o ammonium lau a e,
n-oc anol and wa e . The main conclusion was ha
he ac i a ion ene gy o iscous low o he
he mo opic liquid c ys al u ned ou o be one
o de o magni ude highe han ha o he lyo opic
mesophase (Tamamushi e al, 1976). Di e en
ypes o phospholipids and 2-monoglyce ides o
in e media e chain leng h o m lamella s uc u es,
whe e hyd oca bon chains exhibi a so o luid-like
diso de due o he weakness o he an de Waals
o ces compa ed o he mo ion caused by he mal
ene gy. This is compensa ed by a ac ion o ces
be ween pola heads, gua an eeing he con inuous
exis ence o he bilaye s uc u e (Chapman, 1982),
(La sson, 1994).
GEL PHASES
Gel phases may be ound when c ys als o
amphiphilic lipids a e hyd a ed so ha wa e
eaches he hyd ophilic egion o he bilaye and
he c ys als swell, keeping he c ys alline s uc u e
o he bilaye and he «all- ans» con o ma ion o
he chains (La sson, 1994). The s uc u e consis s
o al e na ing «solid-like» hyd oca bon bilaye s
and wa e laye s. Dialkyl lipids like leci hin p esen
a pa allel a angemen o ails which a e no
inclined, while monoglyce ides a ou bilaye s wi h
a ce ain il . Fu he mo e, po assium s ea a e
o ms monolaye s wi h in e digi a ing hyd oca bon
ails (Tiddy, 1980), (Tiddy and Walsh, 1983). A
good desc ip ion o gel phases o med by
soap/wa e sys ems was p o ided by Winso
(1974). Al e na i ely, his s uc u e may occu
when he lyo opic lamella mesophase is cooled
below he ansi ion empe a u e o he c ys alline
s a e. This ansi ion may be de ec ed by a change
in ei he he quali a i e shape o he sample
iscoelas ic spec um o he quan i a i e alues o
he iscoelas ic unc ions, such as he s o age
modulus, he loss angen , he ins an aneous
compliance, e c. Ekwall (1975) also claimed ha a
so o gel phase may be p oduced when a s i
hyd oca bon skele on, like ha o choles e ol, is
solubilized in a lyo opic mesophase.
While, in some cases, such as he e adecylamine-
wa e sys em (La sson and Al-Mamun, 1974), gel
phases a e conside ed he modynamically s able, in
o he s he gel is me as able e ol ing o a mix u e o
wa e and hyd a ed c ys als o he amphiphilic lipid,
he so-called coagel. Howe e , Laughlin (1990),
(Laughlin e al, 1990) claimed ha he gel «s a e»
should no be ega ded as a disc e e phase, bu i
p obably consis s o colloidally s uc u ed biphasic
mix u es o an o de ed phase (c ys al hyd a es) and
a liquid phase.
The gel s uc u e ep esen s an in e media e
s a e be ween a liquid c ys al wi h i s agg ega es o
uno de ed hyd oca bon ails in a semi luid s a e and
he c ys alline s a e wi h o de ed chains (B own and
Wolken, 1979). I should be no ed ha sa u a ed
diacyl-phospha idylcholines show an in e media e
s uc u e be ween he gel phase and he lamella
mesophase upon inc easing empe a u e, he so-called
ippled phase (La sson, 1994).
LYOTROPIC LIQUID CRYSTALS
Lyo opic liquid c ys als a e o med when pola
sol en s like wa e o glyce ine a e added o
amphiphilic lipids in ce ain composi ion anges.
Su ac an s in dilu e aqueous dispe sions may
assemble in o a a ie y o micella agg ega es
abo e bo h a c i ical concen a ion and empe a u e,
exhibi ing di e en geome ical shapes. These a e
con olled by geome ical cons ain s and by he
in e ace cu a u e, which in u n a e de e mined by
in a-micella o ces occu ing in di e en planes
(Mi chell and Ninham, 1981). As su ac an
concen a ion inc eases in e -micella o ces
become p og essi ely mo e impo an and may
cause ei he a change in he c i ical packing
pa ame e (Is aelach ili, 1985) leading o a u he
shape ansi ion o a diso de /o de ansi ion o he
liquid c ys alline s a e (Tiddy and Walsh, 1983). The
ole o en opic o ces be ween amphiphilic su aces
has also been aken in o accoun by Is aelach ili
and Wenne s öm (1996).
S uc u e o Lamella Liquid C ys als (Lαα)
The mos common lyo opic liquid c ys al has a
lamella s uc u e. In he de e gen indus y, i is
known as he nea soap phase. The molecula
packing in he lamella s uc u e gi es double laye s
wi h he wa e -insoluble ails oge he and he
hyd ophilic pa o he molecule in he bounda ies
wi h wa e . The double laye s pack pa allel o one
ano he and a e sepa a ed om each o he by a
wa e laye . The hyd oca bon chains a e o some
ex en diso de ed, exhibi ing essen ially luid-like
p ope ies and being able o mo e in all di ec ions.
Howe e , his abili y is es ic ed by he in e ac ions
o hyd ophilic g oups wi h wa e .
The s uc u e o he lamella bilaye can be
de e mined by X- ay di ac ion. The hickness o he
wa e laye can a y om ~0.8nm o >10nm depending
on he composi ion, while su ac an bilaye
hicknesses a e gene ally abou 10-50% less han
he leng h o wo «all- ans» su ac an chains
(Tiddy and Walsh, 1983). The hickness dec eases
wi h inc easing empe a u e o wa e concen a ion;
hese changes o hickness may be a ibu ed o he
Vol. 51. Fasc. 1-2 (2000) 9
olding o he hyd oca bon chains and/o he il o
he molecules in he laye s.
This mesophase looks sligh ly anslucen ,
exhibi ing semi- luid p ope ies wi h a weak-gel
heological consis ency, which does no appa en ly
change wi hin i s ealm o exis ence. I is op ically
aniso opic when iewed h ough a mic oscope
be ween c ossed-pola s, showing ex u es clea ly
di e en om hose shown by he hexagonal
mesophase. Lamella liquid c ys alline ex u es may
be homeo opic o ocal-conic ( h eadlike, mosaic o
oily s eaks pa e ns), (Rose ea , 1954), (James y
Hea hock, 1981). While he o me is likely o occu
when a sample is gen ly shea ed be ween he slide
and co e -slip, he mosaic ex u e is enhanced
ei he a high empe a u e o a e ex ensi e
shea ing (F anco e al, 1995). In ac , shea a ou s
disclina ion de ec s in he mic os uc u e ollowing
he low di ec ion (Gallegos e al, 1987a).
In p ac ice, he whole mic os uc u e is
polyc ys alline; i.e. i is o med by he combina ion o
clus e s o lexible bilaye s, each o hem cha ac e ized
by a di ec o which de ines he main o ien a ion o he
so-called monodomain. In o he wo ds, he
polydomain lamella mic os uc u e is o med by
connec ed liquid c ys alline monodomains wi h
andom o ien a ion so ha om a mac oscopic poin o
iew i looks diso ien ed and wi h s uc u al de ec s
(Ba nes, 1980). The echnique o eeze- ac u e
ansmission elec on mic oscopy p o ides clea
pic u es suppo ing he mic os uc u e abo e
desc ibed (Heusch and Kopp, 1987 and 1988),
(Jousma e al, 1987).
The lamella mesophase may be in equilib ium
h ough wo- and h ee- phase egions wi h almos
all he o he mesophases ha occu in amphiphilic
sys ems (Ekwall, 1975). In bina y sys ems he
heo e ically expec ed sequence as wa e
concen a ion dec eases would be: micelles,
lyo opic liquid c ys als (nema ic, cubic, di ec
hexagonal, bicon inuous cubic, lamella , e e sed
bicon inuous cubic, e e sed hexagonal), e e sed
micelles and c ys alline su ac an o he mo opic
liquid c ys al. In p ac ice, no all such possible
ansi ions do occu in eal sys ems.
Rheology o Lamella Liquid C ys als (Lαα)
The pionee ing s udies on he heology o
lyo opic liquid c ys als deal wi h he low p ope ies
o lamella mesophases by de e mining upwa d and
downwa d low cu es, which showed hixo opic
and an i hixo opic beha iou s (Solyom and Ekwall,
1969). Tamamushi (1976) demons a ed he exis ence
o iscoelas ici y in e na y sys ems. Fu he
mani es a ions o iscoelas ici y we e epo ed o a
leci hin/wa e bina y sys em a e de ec ing no mal
s ess di e ences unde shea low, measu ing he
s ess elaxa ion a e s eady low and a emp ing o
conduc small ampli ude oscilla o y shea
expe imen s (Duke and Chapoy, 1976). Bohlin and
Fon ell (1978) p oposed he heo y o coope a i e
coo dina ion numbe o explain he low o he
lamella mesophase. They sugges ed ha shea ing
was likely o c ea e la ge s ongly o ien ed domains
and also claimed ha shea s ess ollowed a
powe -law ela ionship wi h shea a e in mul i-s ep
low cu es, and wi h ime in s ess elaxa ion es s.
The exponen was he ecip ocal o he coope a i e
coo dina ion numbe , which was de ined as he
numbe o s uc u al uni s in e ac ing each o he . An
a e age alue o 2 was p oposed o he lamella
mesophase since i was modelled as lexible
aqueous laye s sandwiched be ween hyd oca bon
bilaye s. This heo y was ex ended o i oscilla o y
shea esul s o lamella and hexagonal mesophases,
al hough no e idence o linea iscoelas ic beha iou
was gi en (Bohlin, 1979). Un o una ely, he whole
heo y has been demons a ed ha ail o explain he
gene al heology o lyo opic mesophases, a leas as
o mula ed by i s au ho s.
The heology o he lamella mesophase o med
by hen-egg leci hin and wa e was s udied by
Bou goin and Shankland (1980). They p oposed ha
p e-shea ed samples exhibi ed a plas ic beha iou ,
eaching a lowes shea a e o abou 0.002s-1. They
con i med he p edic ions o Bohlin and Fon ell (1978)
ha s ess elaxa ion a e s eady shea consis ed o
wo s eps: a nea ly ins an aneous elaxa ion ollowed
by slow s ess decay. Again hey could no conduc
dynamic iscoelas ici y measu emen s in he linea
domain.
Hi sch e al (1982) s udied he low iscous
p ope ies o a lamella mesophase o med in a
qua e na y anionic su ac an /alcohol/hyd oca bon/
wa e o b ine sys em. They epo ed shea hinning
low p ope ies and maximum iscosi ies a
in e media e hyd oca bon concen a ion wi hin he
lamella egion. They also obse ed a d op in
iscosi y wi h bo h empe a u e and NaCl
concen a ion, which was less and less appa en
wi h inc easing shea a es. E en ually a high sal
concen a ion led o he mesophase des abiliza ion
and he mel ing poin o he liquid c ys al was
de ec ed by a ansi ion om shea hinning o
New onian beha iou also con i med by he lack o
bi e ingen ex u es.
Muñoz e al (1988a), (1991) epo ed ha he
Os wald-de Waele powe law indexes o he
lamella mesophase o med by a polyoxye hylene
a y alcohol C12-14EO8we e ha dly in luenced by
ei he concen a ion o empe a u e, al hough a
s eady d op in iscosi y was always ound as
empe a u e app oached he mel ing poin o he
liquid c ys al. Oswald and Allain (1988) we e he
i s o emphasise he ole o s uc u al de ec s in he
10 G asas y Acei es

luid heology o lamella mesophases. In ac , hey
a ibu ed he appea ance o a small peak in
iscosi y a ound he empe a u e loca ing he
lamella /iso opic ansi ion o a ma ked inc ease in
he densi y o disloca ion loops. Paasch e al (1989)
claimed ha he lamella mesophase o se e al
nonionic su ac an s CXEOYo low HLB exhibi ed
yield s esses which we e dependen on he
mechanical p e- ea men o he samples.
A signi ican imp o emen in he heological
cha ac e iza ion o lyo opic liquid c ys als ha e
been obse ed in he nine ies, due o he ac ha
high quali y heome e s we e manu ac u ed a
a o dable p ices and he use o combined s uc u al
and heological echniques. The ansien iscous
low o he lamella mesophase was analysed by
Gallegos e al (1991) and F anco e al (1995). They
asc ibed he s ess decay wi h shea ime no only o
he o ien a ion o liquid c ys alline domains bu also
o hei b eakdown in smalle ones. S a -up a he
incep ion o shea and low in e up ed expe imen s
did no show s uc u al eco e y o he lamella
mesophase a e eaching he s eady-s a e
esponse. In e es ing unde shoo phenomena
occu ing a concen a ions and empe a u es close
o a phase ansi ion we e explained on he basis o
mechanically induced de ec s, which in u n we e
a ou ed by he modynamically s able s uc u al
de ec s. The exis ence o di e en kinds o de ec s in
he lamella mic os uc u e had been p e iously
s udied by se e al au ho s (La Paz e al, 1984),
(Allain, 1985).
McKay e al (1991) epo ed linea iscoelas ici y
esul s ob ained by small ampli ude oscilla o y shea
o he lamella mesophase o med by a double ail
anionic amphiphilic lipid a a composi ion loca ed on
he bo de wi h a dispe sion egion. This ma e ial
u ned ou o be ex emely sensi i e o shea , hence
only below a s ain o 1% a non-des uc i e esponse
was gua an eed and an ins an aneous s uc u al
p obe p o ided. Un o una ely, only was he equency
dependence o he s o age modulus (G', elas ic
componen ) gi en in hei pape . No in o ma ion was
p o ided on he loss modulus (G'', iscous
componen ), p e en ing he linea iscoelas ic
beha iou o his ma e ial om being cha ac e ized.
This wo k was comple ed and imp o ed by (Robles-
Vazquez e al, 1993) since he whole linea
iscoelas ic spec um was gi en and in e p e ed on
he basis o a weak-gel esponse, which implies a
p eponde ance o he elas ic componen on he
iscous one wi hin he s anda d a ailable
expe imen al condi ions. The occu ence o a clea
minimum in elas ici y a in e media e concen a ion
was explained as he esul o a balance be ween an
inc ease in bilaye in e ac ions, ionic s eng h
(sc eening e ec s) and hyd a ion o ces as su ac an
con en ises. The iscous low was desc ibed as
shea hinning, wi h iscosi y being p opo ional o he
ecip ocal o shea a e. I his we e he case, he
shea s ess would no depend on shea a e and
he e o e, his esponse should ha e been ela ed o
a mani es a ion o he sample elas ici y. This can be
con i med upon analysing he esul s ob ained la e , in
a wide shea a e ange, by Al a o (1997), who used
and con olled a e heome e , and Mon al o (1999),
who used a con olled s ess heome e , o lamella
mesophases o med wi h nonionic and ca ionic
su ac an s, espec i ely. Bo h s udies demons a e
ha he shea a e dependence o s ess ollowed a
powe -law ela ionship, a e a c i ical shea a e
alue, exhibi ing simila low indexes (0.5 and 0.6,
espec i ely) highe han he null alues p edic ed by
Robles-Vázquez e al (1993). These also checked
ha he Cox-Me z ule ailed o he lamella
mesophase, as expec ed.
In a u he pape Robles-Vázquez e al (1994)
demons a ed ha upon addi ion o NaCl, he
elas ici y o he anionic lamella mesophase wen
down as shown by he co esponding d op in G'.
This was ela ed o an e ec i e ionic sc eening o
he double-laye epulsi e o ces among bilaye s.
They also a ibu ed a dec ease in G' wi h decane
concen a ion o a so o lub ica ing e ec o his
hyd oca bon inside he hyphophobic moie y o he
bilaye s.
Calaho o e al (1992) epo ed ha , in bina y
suc ose s ea a e/wa e sys ems, he ansi ion
be ween a lamella dispe sion egion and a
monophasic lamella liquid c ys al egion could be
de ec ed by a ma ked all in he c i ical shea a e o
he onse o shea hinning beha iou a low shea a e,
a change in he shea hinning slope and in he
concen a ion dependence o he New onian limi ing
iscosi y a low shea a e. Addi ionally, he occu ence
o a sha p all in he i s di e ence o no mal s esses
(a mani es a ion o non-linea iscoelas ici y) a e
ha ing eached a maximum on he bo de wi h he
dispe sion egion (Figu e 1) was also associa ed wi h
a h eshold concen a ion o he monophasic lamella
egion (Calaho o, 1991), (Gallegos e al, 1994). Such
maximum poin s o he o ma ion o a dispe sion
s uc u e wi h he highes densi y o shea -induced
de ec s. A simila conclusion can be d awn upon
analysing he esul s epo ed by Kilpa ick e al (1994)
o a cesium soap. In his case he onse o he lamella
liquid c ys alline egion can be de ec ed by a ma ked
all o G' wi h su ac an concen a ion a e he
appea ance o a maximum.
Dimi o a e al (1995) demons a ed ha
maximum iscoelas ici y was obse ed a
in e media e composi ion wi hin he ealm o
exis ence o he lamella mesophase in a bina y
nonionic su ac an -wa e sys em. Howe e ,
iscoelas ici y s eadily d opped wi h empe a u e,
anishing a he mel ing poin .
Vol. 51. Fasc. 1-2 (2000) 11
Inc easing/dec easing low cu es de e mined by
Sol e o e al (1995a) on lamella mesophases
o med by an anionic and a ca ionic amphiphilic
lipids, bo h o hem wi h double- ail, may be
in e p e ed assuming ha me as able shea -induced
s uc u es a e o med and e en ually des oyed a
high s ain.
Viscosi ies o he lamella mesophase o med in
a e na y ca ionic su ac an /a oma ic alcohol/wa e
sys em we e shown o inc ease wi h su ac an
concen a ion, al hough his e ec clea ly anished
wi h inc easing shea a es (Mon al o e al, 1996).
The heology o di e en samples loca ed wi hin
he lamella egion o med by a e na y nonionic
su ac an /a oma ic hyd oca bon/wa e sys em was
s udied by Al a o (1997a). Small ampli ude
oscilla o y shea (Figu e 2), c eep compliance and
low cu e esul s indica ed ha he highes le el o
s uc u e was shown by he lamella mesophase a
in e media e bo h mass su ac an /wa e a io and
hyd oca bon concen a ion; i.e. oughly a ound he
cen e o he ealm o exis ence o he lamella
liquid c ys al. This es ic ed zone was associa ed
wi h op imum alues o he c i ical packing
pa ame e o he o ma ion o bilaye s (Al a o e al,
1997b, 1998). The dynamic iscoelas ic spec a
we e in e p e ed in he ime domain by de e mining
he co esponding linea elaxa ion spec a. The
di e en alues o he cha ac e is ic slope o he
pla eau zone ha e been ela ed o di e en
s eng h in e ac ions wi hin and among he lamella
monodomains (Al a o e al, in p ess). In ac , he
weak equency dependence o he s o age
modulus and he low alue o he cha ac e is ic
slope o he pla eau elaxa ion zone may be ela ed
o he o iginal heo y o coope a i e coo dina ion
numbe (Bohlin and Fon ell, 1978). This is possible
by assuming ha he numbe o in e ac ing
s uc u al uni s ends o in ini e ins ead o 2, in
ag eemen wi h he exis ence o a eal
mic os uc u e consis ing o a ne wo k o med by
mic on-sized close-packed liquid c ys alline
domains. A simila hypo hesis has ecen ly been
p oposed o model he linea iscoelas ici y o ood
weak gels (Gab iele e al, 1999).
S ess elaxa ion esul s ob ained in non-linea
iscoelas ic condi ions we e compa ed wi h he
linea elaxa ion spec um de i ed om dynamic
iscoelas ici y. In his way, he s uc u al b eakdown
o he lamella mic os uc u e could be ollowed as
s ain was inc eased by calcula ing a damping
unc ion, which dec eased wi h s ain acco ding o
he model p oposed by Soskey and Win e (1984).
This damping unc ion is use ul o u he modelling
conce ning cons i u i e equa ions (Al a o 1997a).
The impo an ole o he chemical na u e o he
su ace in con ac wi h a lamella mesophase o
unde s and i s heology was i s ou lined by
Ba nes (1980) bu has been comp ehensi ely
s udied by Jage -Léze e al (1998, 1999). While
«solid-like» iscoelas ic esul s we e ob ained on
classical s ainless s eels su aces, non-linea
iscoelas ici y and a « luid-like» iscous esponse
we e obse ed on qua z su aces. These s iking
esul s, which we e suppo ed by small angle X- ay
di ac ion measu emen s, ha e been a ibu ed o
12 G asas y Acei es
0,01 0,1 1 10 100
0,1
1
10
100
1000
10000
G' Filled symbols
G'' Open symbols
(Lα / L1 )
(L1 / Lα )
(Lα )
G',G" /Pa
ω/ ad/s
Figu e 2
Viscoelas ic o mechanical spec a ( equency dependence o
he s o age modulus, G', and o he loss modulus, G'') o a
lamella liquid c ys al, and wo lamella liquid c ys al dispe sions
(Lα/L1: «micella con inuous») and (L1/Lα: «liquid-c ys alline
con inuous»). Measu emen s we e conduc ed on a Haake
Rheos ess RS100 heome e a 25ºC
0 5 10 15 20 25 30 35 40 45 50
0
50
100
150
200
250
300
LAMELLAR LIQUID
CRYSTAL
DISPERSIONS OF MICELLES IN A LAMELLAR
LIQUID CRYSTALLINE MATRIX
11.7 s-1
20.2 s-1
28.7 s-1
106 s-1
165 s-1
σ11-σ22
Suc ose S ea a e Concen a ion (%w )
Figu e 1
Fi s di e ence o no mal s esses, measu ed in a Haake
Ro o isco RV20/CV20N heome e a 50ºC, agains suc ose
s ea a e concen a ion a di e en shea a es
a local alignmen o lamella laye s pa allel o he
su aces a sho dis ances om he qua z pla es,
while in he bulk sample he laye s a e no pe ec ly
o ien ed anymo e. Al e na i ely, his phenomenon
can be analysed as a so o slip e ec on he
qua z su ace. In any case, he ele ance o his
wo k can be be e unde s ood by conside ing he
inc easing popula i y o heome e s, equipped
wi h qua z senso sys ems, o ca y ou pa allel
small-angle ligh sca e ing o small-angle neu on
sca e ing measu emen s, as s a ed by Jage -Léze
e al (1998).
S uc u e and Rheology o Dilu ed Lamella
Mesophases: Lααh, Lααl, Lαα+, L3
Lamella liquid c ys als can be swollen wi h
wa e , al hough la ge swellings a e likely o be
ob ained upon addi ion o hyd oca bons o b ine.
This has been ela ed o he occu ence o
nonelec os a ic epulsi e in e ac ions be ween
highly lexible bilaye s, he so-called undula ion
in e ac ions. These in e ac ions due o he mal
luc ua ions a e conside ed o be esponsible o
he o ma ion o dilu ed lamella mesophases
(Bellocq, 1996). In ac , below 5%w su ac an
concen a ion, esicles, dilu ed bilaye s and
sponge phases can be de ec ed in complex phase
diag ams and a e aising a g owing in e es om
bo h a heo e ical and an applied poin o iew.
Dilu ed lamella mesophases a e likely o appea in
e na y sys ems o nonionic, suga o zwi e ionic
su ac an s, a cosu ac an and wa e (Ho mann,
1994). They ha e also been epo ed o exis ei he
in qua e na y anionic su ac an , cosu ac an , NaCl
and wa e o e en in quina y sys ems (Bellocq,
1996). In addi ion, hey a e also o med in some
bina y sys ems con aining double ail amphiphilic
lipids, like didodecyldime hylammoniumb omide
and wa e . Phospholipids in wa e can o m ei he
uni-o mul ilamella esicles, also called liposomes
(Bó a e al, 1999). In ac , esicles p epa ed om
dipalmi oylphospha idylcholine and wa e exhibi a
leas i e di e en mul ilamella s uc u es in
excess o wa e (Jö gensen, 1995). I is impo an
o poin ou ha phospholipids esicles a e
conside ed as model sys ems o li ing cell
memb anes due o hei simila i ies (Mou i sen e
al, 1995). In addi ion, hey ha e well-known
applica ions in cosme ics bu also in he ood
indus y o mic oencapsula ion o sensi i e
ing edien s (Kim and Baianu, 1991).
Dilu ed lamella mesophases may exhibi
di e en s uc u es. The o ganiza ion o he so-
called Lah phase is simila o classical concen a ed
lamella liquid c ys als since s acks o lexible open
bilaye s a e o med. On he o he hand, he Lal
phase consis s o closed bilaye s ( esicles), which
may be unilamella (Obe disse e al, 1998) o
mul ilamella («onion-like» esicles) exhibi ing a
wide size dis ibu ion (Be gmeie e al, 1997, 1998a,
1998b), (Ma ques e al, 1998). Neighbou ing
esicles may be in closed con ac , sha ing pa o
he bilaye o e en me ging each o he (Ca ia e al,
1998). E en hough a luo ecence dye was used by
Menge e al (1996) o di e en ia e some ypes o
esicles, he mos impo an echnique o ob ain
in o ma ion on he mic os uc u e o hese phases is
eeze ac u e elec on mic oscopy (Ho mann,
1994). In e na y su ac an /alcohol/wa e sys ems,
an inc ease in he cosu ac an concen a ion leads
o a phase ansi ion om esicles (Lαl) o la
lexible bilaye s Lαh(Valien e, 1995).
Phase ansi ions be ween he Lαland Lαhcan be
ollowed by changes in he heology o hese
sys ems. Densely packed mul ilamella esicles a e
likely o exhibi s ong iscoelas ic p ope ies wi h
ex emely long elaxa ion imes due o a high le el
o in e ac ions among hem (Ho mann and Ulb ich ,
1997). Howe e , in some cases, he occu ence o
low-in e ac ing esicles esul s in luid-like iscoelas ic
p ope ies, al hough e en in his case he Lαlphase
exhibi s bo h highe appa en iscosi ies and
iscoelas ici y han he Lαhphase (Ho mann, 1994),
(Mon al o, 1999).
The e ec o shea on dilu ed lamella mesophases
has been ex ensi ely s udied by Roux and
cowo ke s. They p opose h ee main s a es o
o ien a ion depending on he cha ac e is ic dis ance
be ween memb anes as well as he shea a e (Dia
e al, 1993), (Roux e al, 1993) and (Roux, 1997). A
e y low shea a e he bilaye s a e mainly pa allel
o he low wi h de ec s in he wo o he di ec ions.
A highe shea a e o o mo e dilu ed sys ems, he
bilaye s a ange hemsel es in an iso opic s a e
consis ing o closed-packed mul ilamella esicles,
whose size can be con olled by he shea a e. In
ac , he size dec eases as he in e se o he squa e
oo o he shea a e. Panizza e al (1996) ha e
shown ha he pla eau modulus ises as he esicle
size dec eases and enhanced in e ac ions among
he polyhed al esicles ake place. A u he inc ea-
se in shea a e esul s in bilaye s o ien ed again in
pa allel o he low bu wi h no de ec s emaining in
he low di ec ion. The heological esul s we e
suppo ed by a combina ion o se e al echniques:
pola ising mic oscopy, bi e ingence measu emen s,
ligh sca e ing and neu on sca e ing (Dia e al,
1993 and 1995). A simila mechanism seems also
o wo k o semi-dilu ed lamella mesophases as
demons a ed by Laüge e al (1996), who
conduc ed simul aneous heo-small angle ligh
sca e ing measu emen s o a de ec i e lamella
mesophase o a e na y sys em con aining 65%
wa e .
Vol. 51. Fasc. 1-2 (2000) 13
A u he dilu ed lamella mesophase is loca ed
be ween he micella phase and he dilu ed
lamella mesophase in complex sys ems, he
so-called L4o Lα+, which consis s o unilamella o
mul ilamella esicles wi h only a ew laye s. Only
does i show bi e ingence unde low and p esen
luid-like heological p ope ies i unilamella
esicles a e o med. Howe e , high iscosi y and
iscoelas ici y a e obse ed when mul ilaye s
occu (Bellocq, 1996). Fu he mo e, Jons öme
and S ey (1992) epo ed ha he L4memb ane is
mo e igid han hose o he o he dilu ed lamella
mesophases.
Ano he dilu ed phase can be also ound in
complex sys ems as well in bina y sys ems close o
iso opic micella solu ions and swollen lamella
mesophases s abilized by undula ion o ces, he
so-called sponge o L3phase (Mi chell e al, 1983),
(F eyssingeas e al, 1996), (Wagne and S ey,
1999).
Koshinuma e al (1999) ha e ecen ly epo ed a
ansi ion om he sponge phase o unilamella
esicles abo e a c i ical empe a u e and a
subsequen ansi ion o mul ilamella esicles upon a
u he inc ease in empe a u e, in bina y aqueous
sys ems o wo ionic phospholipids: he sodium sal s
o dilau yl- and dimy is oylphospha idylglyce ol.
L3consis s o iso opic phases o andomly
connec ed unen angled bilaye s which sepa a e wo
equi alen egions o sol en s ha ing a Gaussian
cu a u e. In ac , he s uc u e can be desc ibed as
a mol en bicon inuous cubic mesophase (Ho mann,
1994), (Be gmei e al, 1997) so ha he a e age
cu a u e a each poin o he bilaye is ze o since
he wo cu a u es a e conside ed o ha e he same
magni ude an opposi e signs. This phase exhibi s
no signi ican iscoelas ici y and low New onian
iscosi ies a low shea a es bu abo e a c i ical
shea a e a shea hinning esponse is usually
obse ed and a ibu ed o a shea -induced phase
ansi ion o a Lαhphase, whose bilaye s o ien a e in
he low di ec ion (Ho mann e al, 1991), (Mahjoub
e al, 1996), (Mon al o e al, 1998). The sponge
phase has been heo e ically modelled by Ca es e
al (1996).
S able dispe sions may be o med wi h dilu ed
lamella mesophases due o he iscoelas ici y o a
leas one o he phases. Vesicles and ex ended
bilaye s coexis in Lαl/Lαhdispe sions as p o ed by
eeze- ac u e elec on mic oscopy (Ho mann,
1994). In addi ion, he occu ence o s able
dispe sions o a dilu ed lamella mesophase and an
L4phase has been adsc ibed o he high iscosi y o
he la e (Bellocq, 1996). No only a e s able
dispe sions o med in dilu ed sys ems, bu classical
lamella liquid c ys als can also o m highly s able
dispe sions displaying in e es ing heological
beha iou s.
S uc u e and Rheology o Lamella
Liquid-C ys alline Dispe sions
Lamella liquid c ys als can o m s able
dispe sions in bina y as well as in mo e complex
sys ems ou o he «dilu ed» egions. These
dispe sions may be «wa e -con inuous» o «liquid-
c ys alline» con inuous. Alexopoulos e al (1989)
epo ed ha lamella liquid-c ys alline-con inuous
dispe sions o he double- ail anionic su ac an ,
sodium bis(2-e hyl-hexyl)sul osuccina e (AOT) migh
exhibi an i hixo opic p ope ies, a e conduc ing
consecu i e expe imen s in a capilla y iscome e .
The dynamic iscoelas ici y o he same sys em was
ini ially s udied by McKay e al (1991), eaching he
main ollowing conclusions: a) he linea dynamic
iscoelas ic ange was a he small; i.e. he whole
mic os uc u e u ned ou o be ex emely sensi i e o
shea ing o ces, b) once hese dispe sions we e
gen ly shea ed ou o he linea egion, a comple e
s uc u al eco e y could no be checked and c) he
consequence o a ain o inc easing shea a es was
o p omo e an inc ease in G', which could ha e been
in e p e ed as a i s indica ion o a s uc u al build-up
p ocess associa ed wi h a shea -induced
mic os uc u e ansi ion. This was con i med la e by
Valdés e al (1993) ca ying ou inc easing and
dec easing shea a e low cu e expe imen s o he
same bina y sys em.
The exis ence o a phase in e sion in a bina y
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micella con inuous phase and a dispe sion
consis ing o micelles suspended in a lamella liquid
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