JOURNAL OF APPLIED PHYSICS VOLUME 95, NUMBER 3 1 FEBRUARY 2004

Structure-related optical properties of luminescent hetero-opals

N. Gaponika) and A. Eychmuller
Institute of Physical Chemistry, University of Hamburg, 20146 Hamburg, Germany
A. L. Rogach
Photonics and Optoelectronics Group, Department of Physics & Center for Nanoscience (CeNS), University
of Munich, 80799 Munich, Germany
V. G. Solovyev, C. M. Sotomayor Torres, and S. G. Romanovb),c)
Institute of Materials Science & Department of Electrical and Information Engineering, University
of Wuppertal, 42097 Wuppertal, Germany
Received 4 August 2003; accepted 6 November 2003
Light-emitting hetero-opals have been synthesized by successive crystallization of one thin opal film
on top of the other from beads of two different diameters and selective impregnation of one of films
with luminescent CdTe nanocrystals. A strong spectral and spatial anisotropy of the reflectance and
the photoluminescence spectra has been observed and attributed to the photonic bandgap mismatch
in opal films. Changes of the emission anisotropy with excitation power have been associated with
the stimulation of CdTe nanocrystal emission in a host opal film. An interface-related transmission
minimum has been revealed and tentatively explained as the consequence of the distractive
interference of optical modes of hetero-opal constituents. The idea of the interface resonance has
been supported by the observation of the emission modification in this frequency range. 2004
American Institute of Physics. DOI: 10.1063/1.1637135

I. INTRODUCTION and interpretation of specific interface and superlattice phe-

nomena remains ambiguous due to FabryPerot oscillations,
The development of materials inevitably approaches a which are superimposed on reflectance and transmission
phase at which their functionality becomes a merit of the spectra.6 Two cases were theoretically modeled: the plane
progress. With respect to three-dimensional 3D photonic defect in the 3D omnidirectional PhC, which leads to in-gap
crystals PhC, integrating them with efficient light sources interface states,7 and the opal superlattice with several trans-
without deterioration of the photonic bandgap PBG and mission minibands in a PBG.8 However, no results have been
tuning the photon dispersion via insertion of intentional de- reported so far concerning the optical effects associated with
fects are among the most challenging goals. Artificial opals coupling of light at the single PBG interface.
are widely used as 3D PhCs13 in the visible. Because they Recently, we introduced sandwich-type hetero-opals and
are crystallized from colloidal suspensions, it is especially evaluated their optical properties.9,10 In this article, we
desirable to accomplish the formation of opal defects within present the preparation of luminescent hetero-opals impreg-
a self-assembly approach. Otherwise, preparation of opal- nated with CdTe nanocrystals NCs, report the anisotropy of
based functional materials will be dependent on intrinsically their emission properties in conjunction with transmission/
complex nanolithography processing. reflectance spectra, and demonstrate the presence of the spe-
The main idea behind PhC heterostructuring is to obtain cific interface resonance.
an interface, which introduces a sharp distortion in the spa-
tial distribution of the electromagnetic EM field. In spite of
the fact that the geometrical thickness of the interface is II. PREPARATION OF LUMINESCENT HETERO-OPALS
less than the light wavelength, the transition region is formed
Self-assembly of monodisperse latex beads in a fcc lat-
in the vicinity of the interface due to the EM field continuity
tice leads to opal formation.11 Opal films studied in this work
and a need of light coupling from modes of one PhC to
were grown on glass or quartz slides by crystallization of
modes of the other. In this region, which extends over sev-
polystyrene PS beads ranging from 240 to 450 nm in di-
eral lattice periods, one can expect interference between the
ameter D as supplied by Duke Scientific Corporation.
Bloch waves of hetero-PhC constituents.
Aqueous colloidal suspensions of PS beads were carefully
Hetero-opals can be fabricated either by a step-like spa-
washed by two subsequent centrifugations, placed in a Te-
tial infilling of an opal volume4 or by stacking thin opal films
flon cylindrical cell 7 mm inner diameter, and the solvent
of different PBG characteristics.5 However, the observation
was then evaporated under moderate flow of warm air. Weak
vibration induced by air flow was applied to improve the
a
On leave from Physico-Chemical Research Institute, Belarussian State quality of opals in comparison to samples grown by drying
University, 220050 Minsk, Belarus.
b under ambient conditions.12 The optimal quality of the opal
On leave from Ioffe Physical Technical Institute, 194021 St. Petersburg,
Russia. films was achieved in the range of 15 vol % of beads in a
c
Electronic mail: [email protected] suspension. For a given concentration, the average thickness

0021-8979/2004/95(3)/1029/7/$22.00 1029 2004 American Institute of Physics

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1030 J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al.

FIG. 2. Top: Schematics of the LbL coating of the inner opal surface with
polyelectrolyte molecules and CdTe NCs. Bottom: transmission electron mi-
croscope TEM image of 420 nm PS beads, which are LbL coated by CdTe
NCs in one deposition circle. The NCs appear darker due to the higher
FIG. 1. SEM images of a cleaved 300/240 hetero-opal. Thickness of the contrast.
bottom top film is 4.3 6.2 m.

of opal films becomes a function of the suspension volume in bly of polymer-linked NCs.14 This method was applied to a
a cell. Typical thickness of opal films was 510 m. The variety of substrate materials with flat and highly curved
sintering at 90 for 1 h was applied to allow further treatment surfaces.15 Following LbL procedure, the substrate with a
of films. bottom film of a future hetero-opal was immersed for 30 min
Sandwich-type hetero-opals were prepared by self- in a 5 mg/ml aqueous solution of polydiallyldimethylammo-
assembling the top opal film on the surface of the bottom nium chloride positively charge polyelectrolyte, then thor-
opal film, which was crystallized previously from beads of oughly washed and immersed for 30 min in a 103 M aque-
another diameter. Figure 1 shows a scanning electron micro- ous solution of CdTe NCs capped with thioglycolic acid and,
scope SEM image of a hetero-opal, with the bottom film thus, carried a negative charge at appropriate pH. 16 NaCl
consisting of D300 nm and the top film of D240 nm 0.2 M was added to both solutions to facilitate a formation
beads. Here and below, we denote this structure as the 300/ of smooth layers.17 Moderate stirring was applied to solu-
240 nm opal, with the first second number representing the tions to accelerate the mass transfer. NCs 5 nm in diameter
bottom top film. The abrupt interface between them indi- were chosen, because the central frequency of their emission
cates that the formation of the top film proceeds indepen- band in aqueous colloidal solutions18 matches the Bragg
dently on the geometrical profile provided by the bottom PBG of the opal assembled from 240 nm beads. Because
one. This can be due to the fact that the adhesion of the PS opal voids are either of 0.41 or 0.23D in size and connected
beads from colloidal suspensions to the bottom film becomes via 0.15D channels,2 both polyelectrolyte molecules and
weak after the sintering. Primarily, 240/300 nm hetero-opals CdTe NCs can easily access internal pores. We assume that
were optically studied, owing to the similar quality of the the in-void coating proceeds in the same manner as a depo-
interface in hetero-opals with lattice parameter ratios from sition on the open surface. The LbL procedure was repeated
1.12 to 1.87. several times to increase the amount of deposited CdTe NCs.
The layer-by-layer LbL deposition technique, which is The NC/polyelectrolyte layer formed on the opposite side of
based on alternating adsorption of layers of oppositely the slide was finally removed by washing in acetone and
charged species on the surface, was used for impregnation of ethanol.
opal films with luminescent CdTe NCs. LbL technique was The LbL deposition provides uniformity of the coating
originally developed for positively and negatively charged thickness and NC environment Fig. 2, as compared to a
polyelectrolyte pairs13 and was then extended to the assem- direct infiltration of organic dyes19 or semiconductor NCs20

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J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al. 1031

direction. The emission patterns at different frequencies were

extracted from PL spectra measured along several directions
identified by angles with respect to the 111 axis of the
opal fcc lattice. In thin opal films, the mean free path of
photons is comparable to the film thickness; that is, a sub-
stantial portion of the emitted flux of a given frequency
reaches a detector without scattering,21 that allows to observe
the directional nonlinearity of emission.

IV. TRANSMISSION AND REFLECTANCE SPECTRA

OF HETERO-OPALS
The PBG characteristics of both opal films in a 240/300
FIG. 3. a Layout of reflectance and transmission measurements in the nm hetero-opal are similar, but the central frequency of the
Bragg configuration; the angle of incidence is equal to the angle of the
reflectance or transmission. b Layout of the photoluminescence measure-
Bragg gaps is scaled in proportion to the bead diameter Fig.
ments. : the angle of incidence and the angle of detection; : the solid 4a. The transmission spectrum of the hetero-opal exhibits
angle of the light collection. two minima at 1.85 and 2.27 eV Fig. 4b. Similarly, the
reflectance spectrum of the hetero-opal is a superposition of
spectra of individual films, but the reflectance from the illu-
into opals. No leakage of NCs from the bottom opal film
minated film dominates the spectrum Fig. 4b. Assembling
back to water takes place during the deposition of the second
the individual films in a hetero-opal does not change the
film, judging from the absence of the luminescence of the
central frequency of their Bragg resonances; that is, opal
background solution. Anchoring of NCs is also required to
lattices retain their periods. FabryPerot oscillations, which
prevent their diffusion to another film of a hetero-opal.
are superimposed on reflectance spectra, prevent more de-
tailed analysis of the weak reflectance features. The relative
III. EXPERIMENTAL TECHNIQUE
full width at a half-height of both reflectance bands in thin
Transmission and reflectance spectra of hetero-opals opal films is about 8%. The experimental value exceeds the
were measured under white light illumination from a tung- 6.3% BG width, which is extracted from the PBG diagram
sten lamp. A 1-mm-diameter collimated beam was directed calculated by a plane wave method for an ideally ordered
on the opal surface under a certain angle of incidence . The opal, due to the finite film thickness.22 In transmission, the
reflected transmitted light was collected in specular relative BG width is broadened to 9% due to the stronger
straight configuration within a solid angle of approximately influence of light scattered at opal defects. The PBG map of
2 Fig. 3a. It is important to choose the aperture of the the hetero-opal Fig. 4c shows that diffraction resonances
collecting optics to be less than the Bragg cone, which is the on sets of 111 planes follow the Bragg law along the
solid angle covered by the diffraction resonance at a given changing observation angle and do not overlap. The attenu-
frequency, in order to estimate the correct bandwidth of the ation minima are seen down to 60, indicating a good
resonance. Reflectance measurements were performed with ordering of lattices in both opal films.
either the one or the other hetero-opal side facing the detec- An additional transmission minimum can be seen in the
tor to catch the anisotropy. frequency range between Bragg gaps of opal films along the
For the sake of clarity, we will identify the opal film 111 axis at 1.99 eV, if the thickness of the 240/300 hetero-
impregnated with NCs as a source and the other film as a opal becomes less than 10 m Fig. 5a. Similar minimum
filter Fig. 3b. The photoluminescence PL was excited by was observed in a 300/400 nm hetero-opal Fig. 5b. Ap-
the 457.9 nm line of a CW Ar-ion laser focused in 0.1-mm- parently, this additional minimum is a consequence of sand-
diameter spot. PL spectra were collected within a 5 frac- wiching of two opal films with different lattice parameters.
tion of the solid angle Fig. 3b. The excitation power was The selectivity of the interface transmission minimum along
kept low enough to avoid degradation of CdTe NCs. The PL, the frequency axis manifests its interference origin. The fact
which was measured from filter and source films, is hereafter that interface minimum becomes observable only in thin
referred to as source PL and filter PL, respectively. hetero-opals, points at the limited volume of the hetero-opal,
The PL anisotropy along the normal to the interface where this effect takes place. Evidently, this part of a hetero-
plane was obtained by dividing the filter PL spectrum on the opal stretches along the interface plane. The transverse di-
source one. Analysis of the anisotropy as a function of the mension of the transition part corresponds to the coupling
excitation power was performed in the range from 0.5 to 20 length required for transformation of the EM field structure
mW to assess the nonlinearity of the emission. of one PhC into the structure of another. This dimension is
Assuming that emitters in opal are randomly oriented limited to few lattice periods on either side of the junction.
dipoles radiating on average as a point light source, the di- Interface coupling can be accompanied by the distractive in-
rectionality diagram of the emission intensity can be associ- terference of EM waves possessing the same frequency and
ated, in part, with the Bragg cone. As far as the PL intensity wave vector, but originating from different PhC reservoirs if
along a given direction is concerned, it is a convolution of their phase velocities are opposite. In the case of thick
the isotropic emission pattern of the point source and the hetero-opals, the interface minimum is likely obscured by the
number of opal optical eigenmodes propagating along this scattering or overshadowed due to overlap of the broadened

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1032 J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al.

FIG. 5. a Normalized transmission of 20-m-thick 1 and 7-m-thick

2 240/300 hetero-opals at 0. b Normalized transmission of 30-m-
thick 3 and 6-m-thick 4 300/400 hetero-opals at 0. Arrows indi-
cate the interface minimum.

source and the filter PL spectra are shown in comparison to

transmission spectra at different angles of the light detection
to demonstrate the correlation between the emission mini-
mum and the corresponding Bragg gap. It is instructive to
emphasize the different physical origin of this minimum in
the source and the filter PL spectra. The directional minimum
of the source PL spectrum is a consequence of the lower
FIG. 4. a Schematic PBG diagram of a hetero-opal consisting of beads of mode number available for coupling with emitter within the
different sizes (D t D b ) along the L direction, which corresponds to the
111 axis of the opal lattice in real space. Scaling is applied to both the
bandwidth of the diffraction resonance along a given direc-
frequency and the wavevector axis following the difference of the lattice tion, which decreases the emission probability.21 In contrast,
constants in the top and bottom films. b Transmission spectrum 1 of a the minimum in the filter PL spectrum appears due to the
240/300 hetero-opal at 10 and its reflectance spectra at 15, if either back-reflection of the source radiation from a filter film
the 240 nm bead film 2 or the 300 nm bead film 3 faces the detector. c
Angular dispersion of the Bragg BGs of the 240/300 hetero-opal. within the bandwidth of the filter PBG, which does not affect
the emission source itself. In other words, the origin of the
filter PL minimum is the same as that of the transmission
Bragg gaps. Another possible reason for the formation of the minimum. The diffuse scattering of emitted photons at the
resonant state is the cavity along the interface of two opal interface and in the filter film can be the reason for the ab-
films see Fig. 1, which resembles a sort of resonator. The sence of the source PBG minimum in the filter PL spectrum.
quality of this resonator is expected to be very low in pro- The source and filter emission directionality diagrams of
portion to the overlap of the Bragg gaps at the resonance the 240/300 nm CdTe hetero-opal are shown in Fig. 7. The
frequency. Detailed investigation and modeling of this mini- evolution of the source PL pattern with observation fre-
mum will be reported elsewhere.23 quency reflects the overlap of a point source diagram with
the directional PBG. For example, the minimum in the 2.25
eV diagram corresponds to the emission attenuation in the
V. PL IN HETERO-OPALS
Bragg cone directed along the film normal, whereas at 2.34
A straightforward consequence of the PBG anisotropy in eV, the emission minimum is centered at the 25 due to
hetero-opals is the spectral and spatial anisotropy of the lu- the rotation of the Bragg cone. For the 2.0 eV emission fre-
minescence of CdTe NCs embedded therein. In Fig. 6, the quency, which is below the source PBG range, there is no

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J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al. 1033

FIG. 7. Directionality diagrams of the source circles and filter triangles

PL of 20-m-thick 240/300 CdTe hetero-opal at three different emission
frequencies, which are indicated in panels.

FIG. 6. Spectra of transmission a, source PL b and filter PL c of the To reveal the emission anisotropy explicitly, the filter PL
20-m-thick 240/300 nm CdTe hetero-opal. 240 nm film is a source and 300
spectrum was divided on the source one. The filter-to-source
nm film is a filter. Spectra obtained along different directions are labeled by
the angle . Curves in the panel b are shifted vertically for clarity. PL ratio displays a minimum and a maximum, which coin-
cide the filter and source Bragg resonances, respectively, as
shown by the transmission spectrum after subtraction of the
minimum in the diagram. In turn, the filter diagram exhibits Rayleigh scattering component Fig. 8a. In the range from
the minimum along 40 direction at 2.0 eV. At 2.25 eV, 1.94 to 2.08 eV the intensities of the source and filter PL are
the filter 111 Bragg cone is shifted to 80 and cannot be nearly the same and the ratio spectrum exhibits a plateau.
resolved. Correspondingly, diagrams of the filter PL show The noise at the red edge of the ratio spectrum is the result
almost no changes at frequencies above 2 eV. As a result, the of the low PL intensity of CdTe NCs see Fig. 6c.
emission flow within this frequency range is squeezed to the Increase of the excitation power from 0.62 to 20 mW
surface normal after passing the filter. results in a systematic distortion of the ratio spectrum; the
The relative depth of the PBG-induced minimum in the emission attenuation by the filter PBG remains practically
source angle diagram reaches a factor of 1.51.6 that differs unchanged in contrast to the 1.4 times attenuation decrease
from 2.32.6 times PBG attenuation of the filter emission in in the source PBG Fig. 8b. Moreover, at the low fre-
the 20-m-thick hetero-opal. These values underestimate the quency edge of the source gap the ratio becomes less than
intensity suppression because the diffuse component of the unity, indicating that emission enhancement prevails the
emission flow is superimposed on the ballistic component. emission attenuation. In turn, for intermediate values of the
Assuming that the intensity of scattered photons follows the excitation power, the ratio plateau transforms into maximum
Lamberth law and subtracting, consequently, the II 0 cos between 1.96 and 2.06 eV. The focal point, at which intensi-
component from the measured diagram under the assumption ties of the filter and source PL are alike, appears at 2.06 eV
of equal intensity of ballistic and diffuse fluxes, a twofold Fig. 8c. It is noteworthy that the frequency of the focal
improvement of the modulation depth was obtained. This point corresponds to that of the maximum transmission ob-
estimate demonstrates the tendency, but the actual value of served in between two Bragg gaps of the hetero-opal Fig.
the emission suppression remains unidentified due to the lack 8a.
of knowledge concerning the balance between these two To explain the dependence of the PL intensity ratio on
fluxes at a given frequency, the filter film thickness, and the the excitation power in the source Bragg bandgap, we can
distribution of the CdTe NCs in depth of the source film. refer to the increasing contribution of the stimulated emis-

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1034 J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al.

PBG frequencies changes linearly with the excitation power

and the filter PBG attenuation remains unaffected Fig. 8b.
Transformation of the ratio spectrum between two Bragg
resonances as a function of the excitation power is reason-
able to discuss in conjunction with the anomaly of the trans-
mission spectrum. If the interface transmission minimum is
the result of the interference resonance, a fraction of radiat-
ing NCs can be coupled to these resonance modes. By anal-
ogy to the emission nonlinearity in the source PBG, the ra-
diative recombination of NCs coupled to resonance interface
modes will be accelerated. Evidently, the observed PL non-
linearity is proportional to the number of radiating NCs and
to the quality factor of the resonance. On the one hand, the
interface volume accumulates a relatively small number of
NCs because its transverse dimension spans only over few
periods of the source opal film. On the other hand, the shal-
low interface transmission minimum assumes a prevailing
number of unmodified modes, which are available for cou-
pling in the same frequency range. As the result, the
interface-related emission nonlinearity is weak comparing to
that in the source PBG range. Alternative analysis of the
emission saturation threshold in hetero-opals also supports
the idea of the emission stimulation at frequencies of the
interface transmission minimum.26

VI. CONCLUSIONS

Hetero-opals were synthesized by successive crystalliza-

tion of one opal film on top of the other film using monodis-
perse PS beads of a different diameter. The bottom film was
selectively impregnated with luminescent CdTe NCs by
means of the layer-by-layer deposition technique. The trans-
mission spectrum of a hetero-opal shows two main minima
FIG. 8. a The spectrum of the filter-to-source PL intensity ratio thick line following the difference of the Bragg resonance frequencies
at 0 and the transmission spectrum thin line of the 20-m-thick 240/ of its constituents. Strong spatial and frequency anisotropy of
300 CdTe hetero-opal. b Evolution of the filter-to-source PL intensity ratio the reflectance spectrum of hetero-opals is a straightforward
as a function of the excitation power. Numbers indicate the power in milli-
watts. c The same ratios in the vicinity of the interface transmission mini- consequence of this mismatch of the Bragg resonances.
mum. The emission of CdTe NCs embedded in the source film
demonstrates a strong anisotropy with respect to the interface
plane due to asymmetry of the Bragg gaps in hetero-opal
sion, which is added to the spontaneous emission component films. First of all, this is the anisotropy of the radiation pat-
at PBG frequencies at a cost of suppressing the nonradiative tern, because the emission angle diagram depends on the
recombination. The presence of the stimulated emission in shift of the frequency, at which it is measured, with respect
the total emission flow in the Bragg cone was reported in the to the corresponding Bragg gap. Secondly, this anisotropy
case of single film opals impregnated by CdTe NCs.21,24 appears a function of the excitation power because of the
Such radiation is coupled to PBG inhomogeneous optical emission nonlinearity at frequencies of the source gap.
modes, the group velocity vector of which is directed along Two Bragg gaps in the transmission spectrum of a
the resonance direction, but the corresponding wavevector hetero-opal are accompanied by an interface minimum,
points to the allowed propagation direction.25 The group ve- which is likely associated with the distractive interference of
locities of inhomogeneous modes are much lower as com- counterphase optical eigenmodes of hetero-opal counterparts
pared to modes of allowed bands; that is, longer emitter-field near the interface. The idea of the interface resonance is
interaction time facilitates stronger coupling of NCs to inho- supported by the observation of the emission nonlinearity
mogeneous modes. The consequence of these effective reso- occurring in the range between two Bragg gaps, which is
nance conditions is the acceleration of the radiative recom- reasonable to link to CdTe NCs radiating in interface reso-
bination at source PBG frequencies. Evidently, the filter nance modes. Our interpretation of interface-related phenom-
Bragg gap has no influence on the radiative relaxation of ena given above is tentative, and a more elaborated model is
NCs in the source film and, hence, the emission with filter currently under consideration.

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J. Appl. Phys., Vol. 95, No. 3, 1 February 2004 Gaponik et al. 1035

ACKNOWLEDGMENTS 12
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