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Supra Optical Nonlinearities

(SON) of Methyl Red- and
Azobenzene Liquid Crystal
- Doped Nematic Liquid
Crystals
a a a
I. C. Khoo , P. H. Chen , M. Y. Shih , A.
b c a
Shishido , S. Slussarenko & M. V. Wood
a
Electrical Engineering Department ,
Pennsylvania State University , University Park,
PA, 16802, USA
b
Tokyo Institute of Technology , Japan
c
Institute of Physics, Ukranian Acadamy of
Sciences , Ukraine
Published online: 24 Sep 2006.

To cite this article: I. C. Khoo , P. H. Chen , M. Y. Shih , A. Shishido , S.

Slussarenko & M. V. Wood (2001) Supra Optical Nonlinearities (SON) of Methyl
Red- and Azobenzene Liquid Crystal - Doped Nematic Liquid Crystals, Molecular
Crystals and Liquid Crystals Science and Technology. Section A. Molecular Crystals
and Liquid Crystals, 358:1, 1-13, DOI: 10.1080/10587250108028266

To link to this article: http://dx.doi.org/10.1080/10587250108028266

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Supra Optical Nonlinearities (SON) of Methyl

Red- and Azobenzene Liquid Crystal - Doped
Nematic Liquid Crystals
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I. c. KHOO~,P. H. CHEN~,M. Y. SHIH~,A. SHISHIDO~,

S. SLUSSARENKO' and M. V. WOODa

'Electrical Engineering Department, Pennsylvania State University, University

Park, PA 16802, USA, bTokyo Instituie of Technology, Japan and 'Institute of
Physics, Ukranian Acadamy of Sciences, Ukraine

In nematic liquid crystal films doped with methyl-red dye or azobenzene liquid crystal, we
have observed extremely efficient optically induced director axis reorientation effects, and
refractive index change coefficients 7> 1 cm2/W. The basic mechanisms involved are deter-
mined to be optically induced space charge fields and flow reorientation, order parameter
modification and molecular torques by the photo-excited dopant molecules. These
supra-optical nonlinearities (SONS)enable nonlinear image conversion, optical limiting and
holographic grating formation with pW power lasers.

Keywords: liquid crystal; supra-optical nonlinearity; methyl red; azobenzene liquid crystal;
refractive index change; image conversion; optical limiting

INTRODUCTION
Nematic liquid crystals posses very broadband birefingence and transparency [1,2],
-
spanning the visible to infrared spectrum [0.4 microns 12 microns]. Because of their
easy susceptibility to optical fields, they are also highly nonlinear optical materials. By
far laser induced director axis reorientation gives the largest refractive index change An
for a given optical intensity I, the so called nonlinear index coefficient n2 = An/l. Recent
studies have revealed several interesting effects, including 'photorefractive-like'
refractive index change in dyesr fullerene C60- doped nematic liquid crystals,films [3-
51. Observation of perhaps the largest nonlinear index change mechanism in aligned
methyl-red doped nematic liquid crystal film (81 has also been reported. More recently,
we have observed an equally large nonlinear index coefficient in azobenene liquid
crystals (ALC) doped nematic liquid crystal. In planar aligned films, we found that
holographic index gratings can be efficiently generated by co- as well as cross-polarized
writing beams.

OPTICALLY INDUCED REFRACTIVE INDEX CHANGE.

Consider a standard grating diffraction set up in which two polarized coherent writing
beams are overlapped on a nematic film,which is probed by a polarized reading beam
as shown in Fig. la. If the writing beams are co-polarized, they impart an optical
 2 I. C.KHOO ef nl.
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Intensity Grating

Polarized Pump Beams PolarizcdFumpBepmr

@)

Fig. 1. ).a Schematic depiction of grating formation and probe d i h t i o n fkom the indm
grating induced in a nematic film. b.) Optical Intensity grating formed by interfering
two coherent co-polarizedwriting beams. c.) Optical polarization grating formed by
interking two cohmnt crossed-polarized writing beams

intensity grating onto the nematic film I = I, (1 + cos qx), where q is the grating wave
vector, c.f. fig lb. On the other hand, if the writing beams are orthogonally polarized,
the resulting intensity is uniform over the illuminated area, and instead, a polarization
grating is created, c.f. Fig. lc. The polarization state of the light in the overlapped
region varies from circular, through elliptical to liiear in accordance to the phase
difference between the two coherent writing beams. Using a linearly polarized probe
beam, this set up allows one to distinguish various intensity and reorientation dependent
effects.
 SUPRA-OPTICAL NONLINEARITY 3

The writing beams could change the refractive index (as sensed by the probe) of the
nematic film through a variety of processes. These include:
1. Reorientation by dielectric optical torque -Mop
-
2. Reorientation by photo-excited dopant molecular torque h!&jopant
3. Quadratic Photorefractive effects associated with photo-induced space
-
charge field Esc
4. Flow-reorientation effect due to ionic flows caused by space charge fields
-
andor applied field. The shear torque M flow = [gradient V] f(e, a,...)
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5 . Order parameter change AS caused by trans-cis isomerization of the

photo-excited dopant molecules

In purely dielectric non-absorbing nematic liquid crystal, director axis reorientation is

caused by the torque Mop originating &om the dipolar interaction between the dielectric
anisotropy A& and the optical electric field. This effect was first discovered almost two
decades ago, and was termed Giant Optical Nonlinearity (GON)then. The observed n2
values in planar or homeotropic samples are on the order of cm2/Watt. If the
nematic liquid crystals are doped with some dyes capable of excited-state
conformational changes, s t u d i e ~ [ have
~ ~ ~ shown
] that the excited dye molecules could
exert an intermolecular torque M, of much larger magnitude than Mop, resulting in a
nonlinear index coefficientsn2 of cm2/W.

-
PHOTOREFRACTIVE EFFECT Space Charge fields, flows reorientation
Photorefractive-like nonlinearity occurs in nematic liquid crystals lightly doped with
charge producing agents I 3 4 such as Fullerene C60 For a 25 pm thick
homeotropically aligned film under a dc bias voltage of 1.5V,the observed nonlinear
coefficient n2 is in the range of - cm2/W. At the time of its observation, it
was ranked as the largest among all known nonlinear optical materials. The basic
mechanisms are illustrated in Fig. 2. An incident optical field excites the doped liquid
crystals to form charge transfer complexes (CTC). The CTCs subsequently
dissociate[5~9]and create dc space charge fields through ionic diffusion, migration and
other electrodynamicalprocesses. The space charge fields Esc, in combination with an
applied dc field Edc, cause director axis reorientation via the quadratic field effect, i.e.,
the reorientation is proportional to EE.
 4 I. C. KHOO et ul.
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Fig. 2. Schematic depiction of photo-induced space charge field formation in

nematic liquid crystal illuminated by sinusoidal laser intensity. Upper
diagram: along the beam propagation direction. Lower diagram: along the
grating direction.

For an incident optical intensity grating fhction of the form Iop= I0(l+nicosq~),the
photorefractive-like space charge field it is given by:

where kb = Bottzmann constant, cr = illuminated conductivity, a d = dark state

-
conductivity, v = (D+ D-)/(D+ + D-), where D+ and D- are the diffusion constants for
the positively and negatively charged ions, respectively. m is the optical intensity
modulation factor, q = 2 d A is the magnitude of the grating wave vector and 5 is the
coordinate along the grating wave vector.
 SUPRA-OFTICAL NONLINEARITY S

Note that there is a 7112 phase shift between the incident optical intensity function and
the photorefractive space charge field (and the resultant refractive index change). This
phase shift is responsible for two-beam coupling effect in which there is unidirectional
flow of energy from one beam to the ~ t h e r [ ~ * l ~ ] .

TWOother sources of space charge fields arise from the conductivity and dielectric
anisotropies of the nematic under the action of the dc bias field 111:
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(€1, -el)sinecostl
E& = Edc cll sin 28 + cl cos20

where (u//- al)is the conductivity anisotropy and (E// - ~l)

the dielectric anisotropy
of the liquid crystal, and 0 is the reorientation angle.

In addition to this field-induced director axis reorientation effect, the shear torque
associated with the flow of the charged ions and complexes under the dc space charge
fields and the applied dc field also contributes to enhancing the reorientation initiated
by the space charge field. Under continuous illumination, we observed that these flows
induced reorientation is the principal mechanism leading to a very large director axis
reorientation in the steady state.

In the transient domain, when the reorientation angle is small, flows and the Cam
Helfiich field effects may be ignored, the reorientation angle €lo induced in conjunction
with an applied dc field for the configuration as depicted in Fig. 2c is given b y [ 3 ~ ~ ] ,

Since Esc varies as q, therefore €lo- q/[r2/d2 + q2] and it reaches a maximum at a
grating spacing Amax -2d. On the other hand, in the long time case where the
reorientation angle is large, and flows and Can-Helfiich effects are appreciable, the
reorientation angle accounting for all the space charge fields, flows induced
reonentation ....etc. is given by [4]:
 6 I. C. KHOO et al.

e= &E,Esc (O)COS(P)
(4)
A&E:
K[$+q2]+ 4n[l +(A+, +Au/o~)cos(p)+a~Au~~/(~~u,A~)]

Using typical values [1,3] for K, AE, el, Au, u2, a3,112, etc., the second tam in the
denominator is estimated to be on the order of Kx2/d2. In other words, we have
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Notice that in this case, corresponding to long term illurnin?ion of the sample by the
writing beams, the maximum orientation will occur if the grating spacing Amax 0.717-
d. Both relationships (3) and (5) have been verified in our studies of transient and
storage gratings in C40 doped nematic liquid crystal films [31.

SUPRA-NONLINEARITY IN METHYL-RED DOPED NEMATIC LIQUID

CRYSTALS
Recent in methyl-red doped nematic liquid crystal [MRNLC] films
have ushered in the era of supra-nonlinearity. Without the need for a dc bias field, a
-
nonlinear index coefficients 112-10cm2/Wan [x(3) 300 esu], that is lo' times larger
than the previous record. was obtained in standard grating diffraction experiments, c.f.
Fig. 1. The effect is attributed to director axis reorientation caused by the photo-induced
space charge fields in these films. The high photocharge pmdwtion efficiency in
MRNLC is manifested in a sizable dc photo-voltages detected across the IT0 coated
windows, C.f. Fig. 3. LargCr aniSOtropieS A&, U-Ud, V', AUdc, &&..etC, C.f. CX@OnS 1
-2, may also play a role.

A measure of the internal dc apace charge field strength may be obtained from the
dependence of the probe diffraction on an applied dc voltage across the 25 pm hick

field strength of - -
nematic film. From Fig. 4, note that a dc voltage on either direction of lVolt, i.e., a
400 Volthn, completely diminishes the effect, implying that the
internal field along the z-direction is on this order. The field strength between the
grating maxima and minima is even larger, since the intensity contrast is much higher
beween the intensity maxima and minima, than between the two cell windows. In other
word, for comparable grating spacing and thickness, the field along the grating wave
vector is the dominant one.
 SUPRA-OPTICAL NONLINEARITY 7

5.0 _I

-
A

3.0

,
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2.0

I .5

1.o

0.5

0.0
0 50 1 0 0 1 5 0 2 0 0 2 M 3 0 0 3 5 0 4 w 4 5 0 s w 5 5 0

Optical power (WW)

Fig. 3. The dependence of photo-voltage from a 5% Methyl-d doped homeotropic

aligned 5CB film on the optical power for normally and obliquely incident light.
Beam diameter: 9 mm. Sample thickness: 20 pm.

070 ~

065. 0

0
0
0
0

050
0
0 0

a
035-
0
030 - 0

025i 1 I I . I I I 1 I I I 1

"*) N)
Fig. 4. The dependence of the diffraction efficiency &om a 5% Methyl-red doped
homeonopic aligned 5CB film on the optical power for obliquely incident extra-
ordinary writing and probing beams. Sample thickness:20 pm.
 8 I. C. KHOO et a1

That the effect is due to director axis reorientation is confirmed by polarization

dependence of the diffraction, temperature dependence, and the relaxation times [6]. In
general, the reorientation is along the direction of the grating wave vector, and is
independent of the Writing beam polarization for normally incident writing beams
[P=O]. For example, consider the geometry shown in Fig. 3. If the polarization of pump
beams is 0- or e-, and grating wave vector is along x, the director axis orientation is
along x, and only e-polarized probe will yield d i k t i o n . Temperature dependence of
the photovoltage and diffraction also confirm that under the low writing optical
intensity used, there is negligible contribution from thermal effect [ 141.
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There is, however, a notable difference between h4RNLC and photorefractive nematic
liquid crystals. While they share the commonality of photo-charge and -voltage
production, there is. however, no phase shift between the optical intensity function and
the resultant spatial index change created in MRNLC,in contrast to the orientational
photorefiactive effect. Many attempts to observe beam coupling effects in MRNLC
have so far yielded null effect. This and the fact that the reorientation is always along
the grating wave vector have led us to conclude that flow-reorientationeffect also plays
a significant role in this case, c.f. discussion following equation (5). The space charge
fields causes flows of the charge carrying dopant and liquid crystal molecules, creating
shear torque that in tums reorients the LC director axis. In fact, we have observed
similar dependence of the difhction efficiency on the grating constant as the
orientational photorefiactive effect; the difiaction efficiency is maximal when the
grating constant is twice the sample thickncss[3,6]. In a later publication, details of the
calculation and analysis of the experimental results will be given.

Contribution from Trans-Cla Isomerizlmtlon, order parameter change and

molecular torques ?

Since methyl-red arc azo-dyes, they will undergo trans --> cis isomerization, c.f. Fig. 5.
It is well known that the cis species an structurally incongruous with the nematic order
and therefore induce a local disorder at the light intensity maxima [15,16]. The
resulting director axis reorientation is therefore random, and thus both polarization state
of the probe laser will yield dimaction, as the following section on similar grating
-
dimaCtion experiment in ambenzene liquid crystal (AZOLC) doped nematic films
will show. As pointed out in the preceding section, in methyl-rad doped nematic films,
we observed that the reorientation occur on1 along the grating wave vector direction in
1
the low optical intensity regime [l mW/ cm 1, and therefore such ‘disorder’ mechanism
is not likely to be the involved. We did observed that at higher optical intensity, (10’s of
2
mW/cm ), the trans-cis isomerization mechanisms do manifest in a manner similar to
those reported in reference [15]. In this case, both polarization state of the probe beam
will yield diffraction.
 SUPRA-OPTICAL NONLINEARITY 9

Fig. 5. Trans-cis isomerization of AZO -molecules upon optical illumination.

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One possibility that could occur even at low light intensity is the molecular torque
exerted by the photo-excited dye molecules on the NLC. That this mechanism does play
a role is clearly demonstrated in experiments using an input polarization grating on
planar sample. In the case of planar sample with one hard anchoring surface and one
soft anchoring surface, it is found that the methyl-red surface alignment on the soft
anchoring surface could be modulated by such polarization grating, in which the optical
intensity is spatially uniform. Because of the presence also of a z-component dc space
charge field, it is observed that prolonged illumination of the sample lead to permanent
surface realignment, i.e., a permanent grating, as the excited dyes are adsorbed on the
window surface [ 12,131.

AZOBENZENE LIQUID CRYSTAL DOPED NEMATIC NONLINEARITIES.

We have conducted a series of experiments using an azobenzene LC, 4.4 butylmethoxy

ambenzene (BMAB), as a dopant, and in the process, ‘discovered‘ another supra-
nonlinear nematic liquid crystalline material. AZOLC is known to exhibit very well
defined Trans-Cis isomerization process [16] under photo-illumination. The absorption
spectrum of BMAB is shown in Fig. 6. The absorption maximum near 350 nm
corresponds to a I - n+ transition whereas the absorption peak near 450 nm is due to a
n -n* transition. Under illumination by a linearly polarized laser [A = 488 nm]. the
AZOLC molecule will tend to realign with its transition moment along the optical
electric field in order to minimize the energy,

When BMAB is dissolved in the nematic host, and the resultant sample is exposed to
the polarized writing beams, we observe that there are two main mechanisms for
creating director axis reorientation and refractive index change. One is due to Trans -
Cis isomerization. The Cis species are incongruous to the nematic order, and thus
causes order parameter change, and therefore refractive index modification. We found
that at high illumination intensity 10’s of mW/cm2], sufficient Cis species will be
-
created to cause nematic isotropic phase transition. The other index changing
mechanism is the tendency of the Trans molecules to align with its transition moment
perpendicular to the optical polarization [i.e., the long axis parallel to incident light
polarization] in order to minimize the interaction (absorption) energies. This dye
molecular realignment causes the NLC director axis to follow.
 I. C. KHOO et al.

20 r A

15

10
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0.5

00
300 400 50 D 600

Wavelength (nm)

Fig. 6. Absorption spectra of Trans and Cis species of the szobenzcnc liquid crystals in
isotropic phase. Insert is the molecular structure.

Using Fig. 1 set up, we have studied these director axis reorientation effects and
index changes. The following is a summary of the observation and analysis. Planar
samples of AZOLC doped 5CB or E& nematic liquid crystals are made with standard
rubbed polymer-coated cell windows. For the mixture to remain in the nematic phase,
the maximum concentration by weight of AZOLC is about 18 % in SCB, and 10 % in
E7. The film thickness used is 10 microns. These dyedoped samples exhibit dichroism.
Typically, the transmission for light polarized along the director axis is about three
times less than for light polarized perpendicularto the director axis.

Optical Intensity Grating. In the case of an imparted intensity grating, we found that
both order parameter change and molecular realignment effect contribute. Probing the
sample with beam polarized as e- or 0-wave yielded dimaction. In general. if the probe
polarization is parallel to the initial director axis direction, it will experience larger
refractive index modification and yield a higher d i h t i o n efficiency. Because of
diffusion of the Cis species from the intensity maxima and to the minima, the induced
grating tends to be degraded. A typical dynamics of the diffraction is shown in Fig. 7a.
The dimaction rises to a peak and then falls to a much smaller steady state final value.

Optical Polarization Grating. The diffision and grating degradation problem is

eliminated if an optical polarization grating is used. In this m e , uniform intensity
means that the order parameter change is also Uniform. i.e., no grating arise kom this
mechanism. Therefore, the director axis reorientation is due to the moleciilar torqiie
exerted by the illuminated trans AZOLC molecules, which tend 10 align parallel to the
 SUPRA-OPTICAL NONLINEARITY 11

optical field polarization vector as we explained earlier. These molecular torques

reorient the nematic director axis. Since there is no intensity grating in this case, grating
degradation due to diffusion is not present, and the d i m t i o n signal usually could build
up to a large steady state value, as shown in fig. 7b. We do note that at high intensities
(10's of d c d ) , the polarization grating will be wiped out because the whole sample
turns isotropic due to sufficient concentration build up of the cis species.
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Fig.7. 9.) Oscilloscope trace showing the dynamical behavior of the fust order probe
diffraction from the AZOLC doped nematic film induced by an optical intensity
gratmg. Sample thickness: 10 pn. Probe polarization parallel to initial director axis
orientation. b.) Oscilloscope trace showing the dynamical behavior of the f d order
probe diffraction h m the AZOLC doped nematic [SCB] filminduced by an optical
polarization grating.

We close this section with an estimate of the nonlinear index coefficient of AZOLC
doped NLC film. We observed that the best diffraction efficiency is obtained if the
writing beam is normally incident on the planar sample, with the NLC director axis at
45 degrees to the x-axis. In this case, we get a diffraction efficiency of q = 1 % for a
writing beam intensity of 1 mW/cm2 from a 10 micron thick sample. Since q =
( ~ A n d / l ) ~we
, get An = ZxlO', and therefore a nonlinear index coefficient n2 = 2
cm2/Watt. With some optimization, much higher values of n2 could be obtained.

Nonlinearity of Nematic Liquld Crystpls

The nonlinear coefficient n2 of nematic liquid crystals and other well-known nonlinear
optical materials [ 17-19] are listed in Table 1.
 12 I. C. KHOO et al.

Table 1. Refractive Index Coefficients ofNonlinear Optical Materials

Material and Nonlinearities order of magnitude n2 (cm2/W)

Nematic Liquid Crystals

Purely optically induced [ref.I ] ............
Excited dye molecular torque [ref.l3] ..........10-3
Photorefiactive -C60 doped [ref.l4] ............. 10-3
.................... 10
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Isotropic Liquid Crystals [

GaAs bulk rref.171 ................................................ 10-5
GaAs MQW [ref.18] .........................
Photorefractivecrystals [ref.191 .......
CS2 [ref.l] ........................................

These supra nonlinearities have been utilized for image processing with pW/cm2
intensities, and optical limiting application with hi& dynamic range [141, following our
previous observation of self-defwusing and optical limiting effect with nanowatt powef
laser [20]. An attractive feature of such imaging conversion process using MRNLC
film is that visible image can be reconstructed with an input beam intensity as low as 70
pWan/cm2. This sensitivity is among the best of all known optical processing materials,
and rivals those obtainable from commercial [and much more expensive] liquid crystal
spatial light modulator LCSLM[21*22]used in adaptive optics systems.

CONCLUSION
In conclusion, nematic liquid crystals in its various pure and doped forms possess many
interesting nonlinear optical responses. In methyl-red or azobenzene liquid crystal
doped nematic films,we have observed suprasptical nonlinearity characterized with
index coefficients that are orders of magnitude larger than all known nonlinear optical
materials.

ACKNOWLEDGEMENT
This work is supported by the Army Research Office and Joint Services Agile Program.
We greatly appreciate Prof. T. Ikeda of Tokyo Institute of Technology for providing the
azobenzene liquid crystal.

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