The electro-optical and electrochromic properties of electrolyte-liquid crystal

dispersions
Daniela Cupelli, Giovanni De Filpo, Giuseppe Chidichimo, and Fiore Pasquale Nicoletta

Citation: Journal of Applied Physics 100, 024515 (2006); doi: 10.1063/1.2219696
View online: http://dx.doi.org/10.1063/1.2219696
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The electro-optical and electrochromic properties of electrolyte-liquid
crystal dispersions
Daniela Cupelli, Giovanni De Filpo, and Giuseppe Chidichimo
Dipartimento di Chimica, Universit della Calabria, 87036 Rende (Cosenza), Italy
Fiore Pasquale Nicoletta
a
Dipartimento di Scienze Farmaceutiche, Universit della Calabria, 87036 Rende (Cosenza), Italy
Received 25 November 2005; accepted 14 May 2006; published online 31 July 2006
Liquid crystals are known to exhibit a reversible color change by applying a direct current electric
eld, if a small amount of quaternary ammonium salts is dissolved into them. Applications of such
an electrochromic liquid crystal cell have been proposed as interesting laser-addressed writing and
image storage devices. Liquid crystal dispersions are composite materials formed by liquid crystal
droplets embedded in either a polymer or a monomer matrix. Thin lms of liquid crystal dispersions
can be turned from an opaque to a transparent state by application of a suitable alternating current
electric eld. Herein, we report our investigations on electrolyte-liquid crystal dispersions, which
show independent electro-optical and electrochromic properties characterized by fast bleaching
times. This cell involves the reorientation of liquid crystal molecules, trapped in droplets, for the
electro-optical changes from the opaque to transparent state and the formation of complexes at the
cathode, between the positive ions of electrolyte and liquid crystal dispersed in the matrix, for the
electrochromic changes from the bleached to colored state. The device is able to change its
electro-optical transmittance within few milliseconds and its color within few seconds. 2006
American Institute of Physics. DOI: 10.1063/1.2219696
I. INTRODUCTION
Organic electrochromic materials are being widely in-
vestigated for their variety of colors, which allow interesting
applications such as light shutters, smart windows, and ac-
tive displays.
16
These materials include bipyridilium sys-
tems, conducting polymers, quinones, phthalocyanines,
terephthalates, and cyanobiphenyls.
1
These latter materials
with a small amount of electrolyte exhibit a reversible and
intense color change, if a direct current dc electric eld is
applied or removed.
7
The interest in electrolyte doped cyano-
biphenyls resides in the fact that they are components of
liquid crystal mixtures now widely used in electronic de-
vices. When a dc electric eld is applied to an electrochro-
mic liquid crystal cell ECLC, i.e., a liquid crystal doped
with small amount of electrolyte e.g., tetrahexylammonium
iodide, THAI sandwiched between two conductive glass
substrates, colored species are produced at the cathode.
Nakamura et al.
8
have proposed a mechanism for the
coloration in ECLCs, which involves, when the dc electric
eld is turned on, the migration of positive ions of electro-
lyte, THA
+
, to the cathode and the formation of colored
charge transfer complexes between them and cyanobiphenyls
reduced at the cathode. The bleaching occurs when the dc
eld is removed and is attributed to the diffusion of halide
molecules, I
2
, produced by oxidation at the anode and their
reaction with colored species. The electrochemically induced
color depends on the type of used liquid crystal, i.e., on the
type of terminal group forming the component. In particular,
4-cyano-4-n-alkylbiphenyls and 4-cyano-4-n-alkoxy-
biphenyls nCB and nOCB of general formula
C
n
H
2n+1
C
6
H
4
C
6
H
4
CN and C
n
H
2n+1
OC
6
H
4
C
6
H
4
CN, respec-
tively and chiral nematic biphenyls such as C15 and CB15
of molecular formula C
2
H
5
CHCH
3
CH
2
OC
6
H
4
C
6
H
4
CN
and C
2
H
5
CHCH
3
CHC
6
H
4
C
6
H
4
CN give colored cells,
which appear bluish green to the eye. On the contrary,
alkoxy-benzylidene cyanoanilines general formula
C
n
H
2n+1
OC
6
H
4
CHNC
6
H
4
CN give an orange coloration. If
a eutectic mixture is used, the resulting color will bej the
superimposition of all single colorations due to each
liquid crystal component. The main drawback is that the
composition of most eutectic mixtures is unknown, being
under patent. So it is not possible to predict the nal color
of cells. The compositions of E7 nematic liquid crystal
are 51 wt. % 5CB, 25 wt. % 7CB, 16 wt. % 8OCB, and
8 wt. % 5CT a cyanoterphenyl of molecular formula
C
5
H
11
C
6
H
4
C
6
H
4
C
6
H
4
CN and, experimentally, give rise to a
green coloration. E49 nematic mixture, which has chemical
physical properties similar to those of E7 but unknown com-
position, gives a yellowish green color upon application of a
dc electric eld, if it has been doped with ammonium salts.
The origin of electrochromism can be attributed to the for-
mation of colored complexes between the phenyl rings and
ammonium ions, as reported by Nakamura et al.
9
In that
work, the authors investigated the electrochromic behavior
of organic materials with relatively simple molecular struc-
ture. All compounds had a common phenyl ring and different
terminal groups. They found that the electrochemically in-
duced color depends upon the type of terminal groups and
their position para, meta, ortho in the compounds.
The electrochromism is observed both in liquid crystal-
line state as well as in the isotropic state. Nematic, smectic,
a
Electronic mail: ore.nicoletta@unical.it
JOURNAL OF APPLIED PHYSICS 100, 024515 2006
0021-8979/2006/1002/024515/5/$23.00 2006 American Institute of Physics 100, 024515-1
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and cholesteric ECLCs have been investigated
7
even if their
electrochromic properties are lowered by resistivity increase
and texture changes due to electrohydrodynamic instabilities.
Nevertheless a laser addressed smectic liquid crystal light
valve with electrochromic properties has been proposed.
10
The study of time dependence of the coloration and
bleaching after the application and removal of the dc eld
led to rather simple equations, which well tted the experi-
mental results. In particular, the coloration density increases
linearly with the current, and the dominant electrochemical
reaction for bleaching is a rst order one.
Liquid crystal dispersions are composite materials con-
sisting of micrometer sized liquid crystal droplets dispersed
either in a solid polymer matrix
11
polymer dispersed liquid
crystals, PDLCs or in a viscous oligomer matrix
12
liquid
crystal emulsions, LCEs. Liquid crystal dispersions can be
turned from an opaque to an optically transparent state by
application of a suitable alternating current ac electric eld.
The operation principle is the electrically driven reorienta-
tion of liquid crystal directors, from their structures and av-
erage orientations taken within the droplets, along a prefer-
ential direction parallel to the external eld. Upon
application of a sufcient electric eld, the reorientation of
liquid crystal droplets leads to a transparent state. An exact
matching between the liquid crystal ordinary refractive index
of liquid crystal droplets and polymer matrix one is desirable
even if not absolutely necessary. PDLCs and LCEs have be-
come a recent focus of research for application such as spa-
tial light modulators, switchable shutters, and displays.
13
In
the past it has been demonstrated that polymer dispersed
cholesteric liquid crystals can be used in electro-optical color
displays
1417
as their helical texture selectively reects a spe-
cic wavelength of light associated with the cholesteric he-
lical pitch, when light propagates parallel to the helical
axis.
18
More recently, we have shown that liquid crystal disper-
sions hosting electrochromic guest molecules are able to give
both an independent and fast switching from a scattering
opaque state to a transmissive transparent state, owing to
liquid crystal director reorientation, and a color change, due
to electrochromic reactions occurring at the electrodes.
19,20
Both changes are obtained with rather fast switching and
relaxation times: few milliseconds and few seconds for the
electro-optical and electrochromic responses, respectively.
Bifunctional devices that possess both the electrically con-
trolled scattering and electrochromic properties are important
in practical applications.
Herein, we report our results devoted to fabrication and
characterization of a bifunctional device based on
electrolyte-liquid crystal dispersions ELCDs, in which the
liquid crystal is responsible of both color and transmittance
changes. Both relaxation times remain almost unchanged
with respect to our previous bifunctional devices, but the
preparation process is extremely simplied by using all com-
mercially available materials and offer, in addition, a great
variety of colors.
II. EXPERIMENTAL PART
PDLC lms were prepared by a thermally or
polymerization-induced phase separation process. LCEs
were prepared by mixing liquid crystals and bisphenol A
glycerolate diacrylate in different weight ratios.
12
The nem-
atic liquid crystals used in this work were eutectic mixtures
of cyanobiphenyls E7, E49, CB15, and ZLI4788-000 from
Merck and TN10427 from Rolic. Thermoplastic matrices
were polymethyl methacrylate, polyisobutyl methacry-
late, and polyvinyl butyral from Aldrich. PDLCs were ob-
tained via polymerization-induced phase separation starting
from LCE doped with small amounts of either thermal or UV
initiators 2 wt. % azoisobutyronitrile from Aldrich and
2 wt. % Irgacure 651 from Ciba, respectively.
Ammonium salts tetrabutylammonium tetrauorobo-
rate, tetrabutylammonium hexauorophosphate, tetrabuty-
lammonium perchlorate, octadecyltrimethylammonium bro-
mide, and didodecyldimethylammonium bromide all from
Aldrich were dissolved in different weight percentages
from 1% to 25% in propylene carbonate Aldrich. The
choice of either a particular polymer or ammonium salt can
produce a change in the intensity and shade of the device
color. Bifunctional liquid crystal dispersions were prepared
in vials by mixing the appropriate amounts of polymer or
oligomer 3074 wt. %, liquid crystal 6025 wt. %, and
electrolyte solution 101 wt. % in a common solvent. Af-
ter solvent evaporation, a small amount of mixture was sand-
wiched between transparent conductive substrates. The cell
gap was 40 m. Cells were heated to about 100 C and,
then, cooled at a controlled rate untill room temperature in
order to induce phase separation. Alternatively, cells, con-
taining polymerization initiators, were either UV light ex-
posed for 15 min average power of 10 mW/ cm
2
or heated
to 70 C for 2 h. The electro-optical properties of samples
were measured with the optical setup previously reported.
21
Spectroelectrochemistry was performed with a YASCO
V550 UV-vis spectrometer.
In this paper we report results concerning polymethyl
methacrylate based samples. In particular, either E7 or E49
was used, in the weight ratio polymer:liquid crystal =1: 1, for
the preparation of PDLCs, which were doped with different
percentages 2.5, 5, and 10 wt. %, 5 wt. % if not clearly
written of an electrolyte solution tetrabutylammonium tet-
rauoroborate 10 wt. % in propylene carbonate.
III. RESULTS AND DISCUSSION
If the liquid crystal concentration in ELCD is kept below
the onset of phase separation around 2530 wt. % for poly-
methyl methacrylate based devices, small variations de-
pend on the different liquid crystal solubilities, lms appear
to be transparent and uncolored. They do not possess electro-
optical properties as liquid crystal is dispersed in the matrix
and is not phase separated in droplets. Nevertheless, they
acquire different colors as a function of the used liquid crys-
tal if a dc electric voltage 2 V is applied as reported in Fig.
1. The differences in the absorption can come from the dif-
ferent compositions of used eutectic mixtures E7, E49, and
ZLI 4788-000 and from the particular chemical structure of
024515-2 Cupelli et al. J. Appl. Phys. 100, 024515 2006
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CB15 the presence of a chiral center. These lms are really
electrochromic polymeric solid lms. They are self-
supporting and can be subsequently laminated between con-
ductive substrates. Their self-supporting nature provides
many benets to the electrochromic devices manufactured
within, including the enhancement of processibility and,
from a safety perspective, in the event that electrochromic
devices should break or become damaged, the polymer ma-
trix is able to impede seepage in the environment. For the
sake of completeness, samples are not perfectly sealed by
polymer matrix and liquid crystal can seep out of or other
liquids can seep into the cells over time.
The increase of liquid crystal concentration causes phase
separation. Liquid crystal droplets form and increase their
number and size. Electrolyte-liquid crystal dispersions ap-
pear opaque and uncolored when no eld is applied. The
opaque state is a consequence of the random distribution of
liquid crystal directors that scatter light. If an ac external
eld is applied drive frequency
drive
=1 kHz, liquid crystal
directors will reorient along the eld direction, the light scat-
tering will be largely reduced, if the match condition is sat-
ised, and the device will appear transparent.
13
The eld
dependent transmittance of a typical electrolyte-E49 liquid
crystal dispersion E49-ELCD is reported in Fig. 2. There is
no particular effect due to the presence of electrolyte with
respect to conventional PDLCs.
The off state transmittance is around 1% and reaches
80% value when electric eld strength lower than 3 V m
1
is applied the acceptance angle is equal to 2.5. It is impor-
tant to note that, increasing the electrolyte concentration, the
response of transmittance to the applied eld becomes
sharper and shifts towards lower switching elds. This is in
agreement with previous works reporting similar effects due
to an increase of polymer matrix conductivity.
22
Another pos-
sible explanation for these experimental results i.e., the
lms respond at lower electric elds with increasing doping
levels could be a decrease in the clearing temperature of
liquid crystal and a consequent reduction of its elastic con-
stants due to the carrier solvent propylene carbonate. Opti-
cal observations in E7 based PDLCs, with 10 wt. % of elec-
trolyte solution, showed appreciable changes in the clearing
temperature of liquid crystal 56 C rather than 60 C.
If a simultaneous dc excitation 2 V is provided to the
samples, their T vs E curves are slightly right shifted due to
the presence of small depolarization elds. As an example,
curve a changes to curve d in Fig. 2, if one supplies a dc
eld.
If the external eld is removed, the restoring forces act-
ing at droplet interfaces will cause the random distribution of
director orientations within few milliseconds. The electro-
optical response of an electrolyte-E49 liquid crystal disper-
sion is reported in Fig. 3. The driving eld is a square wave
at the drive frequency of 1 kHz and with a rms drive strength
of 3 V m
1
. Both the rise and the decay times are of the
order of few milliseconds. Such values are similar to those
shown by conventional PDLCs. No appreciable changes in
the response times are observed if a simultaneous dc excita-
tion is provided e.g., in Fig. 3 curve a changes to curve d,
which results less noisy.
The increase of electrolyte concentration in samples
causes a decrease in the rise and decay times, due to a faster
onset and depletion of the local elds acting on droplets.
22
The optical properties of electrolyte-liquid crystal dis-
FIG. 1. Absorbance through electrolyte-liquid crystal saturated dispersions
in their dc on state with different liquid crystals: a CB15, b E7, c E49,
and d ZLI4788-000.
FIG. 2. Transmittance dependence on ac electric eld
drive
=1 kHz
through bifunctional electrolyte-E49 liquid crystal dispersions for different
electrolyte solution ES loadings: a ES=2.5%, b ES=5%, c ES
=10%, and d ES=2.5%, with a 2 V dc simultaneous excitation.
FIG. 3. Electro-optical response of bifunctional electrolyte-E49 liquid crys-
tal dispersions for different electrolyte solution ES loadings: a ES
=2.5%, b ES=5%, c ES=10%, and d ES=2.5%, with a 2 V dc simul-
taneous excitation.
024515-3 Cupelli et al. J. Appl. Phys. 100, 024515 2006
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persions were examined by spectroelectrochemistry over the
whole visible range after the application of a dc eld.
Figure 4 shows the changes in the steady-state absor-
bance for E49-ELCDs containing different electrolyte con-
centrations. The absorbance and, consequently, the sample
coloration increase as the electrolyte concentration increases.
If the coloration process is observed at the optical micro-
scope along cross sections of thick samples 2 mm, it is
evident that the colored region grows at the cathode as a
function of dc current time and electrolyte concentration. As
a consequence, the coloration is due to the increase in layer
thickness of colored complexes at the cathode.
The change in the absorbance for samples of Fig. 4 dur-
ing a coloration and bleaching sequence is reported in Fig. 5.
When a dc current is applied to cells, colored complexes
are produced at the cathode. The absorbance reaches a pla-
teau value within few seconds 1216 s depending on elec-
trolyte concentration and dc current application time. Upon
eld removal the color spontaneously bleaches within some
seconds 45 s depending on electrolyte concentrations. It
is important to note that short bleaching times can be ob-
tained by shortening the cells.
The choice of halide counterions does not affect the
color of cells. Similar colorations are obtained by using qua-
ternary ammonium salts with different halides. On the con-
trary, the type of liquid crystal used in the formulations gives
different absorption spectra and, consequently, different col-
ors to the lms as shown in Fig. 6 for E7 curve a and E49
curve b.
Following the mechanism of coloration and bleaching
proposed by Nakamura et al.
8
for the electrochromism of
liquid crystal materials, the application of a dc current to an
ELCD causes the migration of ammonium ions A
+
to the
cathode, where the reaction between A
+
and liquid crystal
LC,
A
+
+ LC+ e

A
*
LCcolored,
takes place and gives a colored complex.
At the same time halide molecules, Ha
2
, are produced at
the anode. These last molecules diffuse and react with the
colored species according to the following reaction:
2A
*
LC+ Ha
2
2A
+
+ LC + 2Ha

uncolored,
determining the bleaching of the sample when the dc exter-
nal eld is removed.
The combined electro-optical and electrochromic behav-
iors of E49-ELCDs were examined by spectroelectrochemis-
try by applying different electric elds, as shown in Fig. 7.
The four distinct states are a opaque and uncolored, when
no eld is applied; b opaque and colored, if a dc electric
eld is turned on; c transparent and uncolored, when an ac
electric eld is applied; and d transparent and colored, if
both the ac and dc electric elds are present.
The opaque state is due to light scattering by liquid crys-
tal droplets, and the transparent one is attributed to liquid
crystal director reorientations as previously reported in other
bifunctional devices.
19,20
Color is a consequence of the elec-
trochromic reactions, which take place at the cathode be-
tween ammonium ions and liquid crystal. The pictures of the
four states are reported in Fig. 8 for an E49-ELCD. Even if
the migration of ions to electrodes is the basic physical prin-
ciple as previously reported,
19,20
different reactions take
FIG. 4. Spectroelectrochemical UV-vis transmittance through bifunctional
electrolyte-E49 liquid crystal dispersions for different electrolyte solution
ES loadings: a ES=2.5%, b ES=5%, and c ES=10%.
FIG. 5. Changes in optical absorbance during a coloration and bleaching
sequence for electrolyte-E49 liquid crystal dispersions with different elec-
trolyte solution ES loadings: a ES=2.5%, b ES=5%, and c ES
=10%.
FIG. 6. Spectroelectrochemical UV-vis transmittance through bifunctional
electrolyte-liquid crystal dispersions for different kinds of liquid crystals: a
E7, and b E49. Sample a looks green and b dark yellow.
024515-4 Cupelli et al. J. Appl. Phys. 100, 024515 2006
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place, i.e., the formation of a colored complex rather than the
oxidation and/or reduction of components. In addition, this
device results to be extremely simplied as the ammonium
salts play a double role of chromogenic material and conduc-
tivity enhancer, and the liquid crystal, which is usually an
isotropic plasticizer dispersed in the matrix, is used as sec-
ond chromogenic molecule. Consequently, the cell does not
need conductive oligomers ad hoc synthesized and redox
couples. Since a high conductivity often degrades the stabil-
ity or the lifetime of PDLCs e.g., by discoloring the in-
dium tin oxide ITO conductive substrates the electrolyte
concentration should be carefully determined depending on
the particular application.
IV. CONCLUSIONS
We have shown that electrolyte-liquid crystal dispersions
represent a class of materials, which are able to combine the
electro-optical properties of liquid crystal dispersions and the
electrochromic properties of electrolyte-liquid crystal mix-
tures. The proposed device is able to change its electro-
optical transmittance within few milliseconds and its color
within few seconds. The lms represent a simplication in
the preparation of bifunctional devices, as they do not need
the use of any particular chemical, such as conductive oligo-
mers, and of other electrochromic molecules, such as violo-
gens. The matrix conductivity is opportunely increased by
the electrolyte solution. The liquid crystal dispersed in the
matrix, which is generally considered a lost material, acts
as chromogenic molecule. Consequently, ELCDs could offer
interesting contributions in the color display production.
Work is in progress in order to obtain ELCDs operating in a
reverse mode, i.e., transparent in the off state and opaque
when an ac electric eld is applied.
ACKNOWLEDGMENT
MIUR, the Italian Ministry for University, is acknowl-
edged for nancial supports Grant Nos. Ex60% and
PRIN2005.
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FIG. 7. The four states of a bifunctional electrolyte-E49 liquid crystal dis-
persion: a opaque and uncolored, b opaque and colored, c transparent
and uncolored, and d transparent and colored.
FIG. 8. Color online A picture of the four states of a bifunctional
electrolyte-E49 liquid crystal dispersion: a opaque and uncolored, b
opaque and colored, c transparent and uncolored, and d transparent and
colored.
024515-5 Cupelli et al. J. Appl. Phys. 100, 024515 2006
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