Received: 22 March 2019 

|   Revised: 10 June 2019 

|  Accepted: 18 June 2019

DOI: 10.1002/ces2.10015

ORIGINAL ARTICLE

Effects of processing parameters on 3D structural ordering and

optical properties of inverse opal photonic crystals produced by
atomic layer deposition

Heloisa G. Campos1  | Kaline P. Furlan2,3   | Daniel E. Garcia1  | Robert Blick3  |

Robert Zierold   3
| Manfred Eich   4,5
| Dachamir Hotza   1
| Rolf Janssen 2

1
Graduate Program in Materials Science
and Engineering (PGMAT), Federal
Abstract
University of Santa Catarina (UFSC), Vertical convective self‐assembly has been extensively used for the preparation of
Florianópolis, Brazil direct photonic crystals, which can be later infiltrated with a more stable material,
2
Institute of Advanced Ceramics, Hamburg
such as oxide ceramics, by atomic layer deposition. However, the relationship be-
University of Technology (TUHH),
Hamburg, Germany tween the self‐assembly parameters of the direct photonic crystals and the optical
3
Institute of Nanostructure and Solid‐ properties of the inverse opal photonic crystals remains elusive. In this work, the
State Physics and Center for Hybrid effect of different experimental parameters on the 3D structure and the density of
Nanostructures, Universität Hamburg,
Hamburg, Germany
defects of polystyrene direct photonic crystals produced by vertical convective self‐
4
Institute for Optical and Electronic assembly was assessed. Self‐assembly was investigated using deionized water as
Materials, Hamburg University of media with polymer particles’ concentrations up to 2 mg/mL; temperatures of 40,
Technology, Hamburg, Germany
50, and 80°C; and relative humidity of 45%, 70%, and 90%. The 3D structure of the
5
Institute of Materials Research, Helmholtz‐
resultant direct photonic materials was characterized by the combination of scanning
Zentrum Geesthacht, Geesthacht, Germany
electron microscopy and image analysis, and their optical properties were assessed
Correspondence by reflectance measurements. These results were correlated with the performance of
Rolf Janssen, Institute of Advanced
Ceramics, Hamburg University of
oxide‐based inverse opal photonic crystals produced by the controlled infiltration of
Technology, Hamburg 21073, Germany. the former direct photonic crystals by atomic layer deposition (ALD). It was found
Email: [email protected] that the thickness increased with the concentration of polystyrene particles, while the
Funding information photonic structure ordering is dependent on the synergy between humidity and tem-
SFB 986 Hamburg University of perature. Results also showed higher defects population with increasing evaporation
Technology, Grant/Award Number:
temperature and decreasing relative humidity.
DXX/3264/SFB/1986/M09/C5

KEYWORDS
3D structure, optical properties, photonic materials, vertical convective self‐assembly

1  |   IN TRO D U C T ION weak forces such as van der Walls, electrostatic, hydrogen
bonds, hydrophobic, and stacking interactions as well as ste-
Self‐assembly is a process whereby individual components ric forces.1 Application of self‐assembly techniques requires
arrange themselves into an ordered structure. In a self‐as- highly ordered photonic crystals, such as optical fibers, la-
sembled structure, the building blocks are usually linked by sers, photovoltaic cells, and other optoelectronic devices.2‒6

This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original
work is properly cited.
© 2019 The Authors. International Journal of Ceramic Engineering & Science published by Wiley Periodicals, Inc. on behalf of American Ceramic Society

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68    wileyonlinelibrary.com/journal/ces2
 Int J Ceramic Eng Sci. 2019;1:68–76.
CAMPOS et al.
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     69

Colloidal crystals can be self‐assembled from a colloidal

suspension by evaporation of the liquid solvent or by grav-
2  |  M ATERIAL S AND M ETHO D S
ity sedimentation in a variety of approaches,7 such as spin
Monodisperse polystyrene (PS) particles (microparticles),
coating,8 vertical deposition,9,10 electrophoresis,11,12 centrif-
with diameter of (0.76  ±  0.02)  µm, were self‐assembled
ugation,13 freezing,14 physical confinement,15 or convective
on single crystal sapphire substrates (25  ×  30  ×  0.53  mm,
self‐assembly16 to name a few of them.
Crystec). Vertical convective self‐assembly (VCSA) was
Vertical deposition is the method most extensively ap-
performed inside a humidity chamber (HCP 108, Memmert)
plied to produce outsized scale colloidal crystals. Novel
for 120 hours, or until the complete evaporation of the solvent
functional nanomaterials such as photonic materials with
using Teflon beakers containing PS suspensions in filtered
tailor‐made thickness have been obtained using a bottom‐up
deionized water. The angle between the substrate normal and
fabrication approach.17‒19 However, depending on the type
the beaker base was kept at 81° to 84°.
and the extent of the defects, colloidal crystals may suffer
Colloidal crystal films were obtained by controlled evap-
from reduced reflectance capability or no photonic band gap
oration of the liquid and different combinations of PS con-
making them unusable for applications.20 Typical defects
centration (1, 1.5, 2 mg/mL), temperature (40, 55, 80°C), and
may include line defects, point defects, drying cracks, stack-
relative humidity (RH) (45%, 70%, 90%).
ing faults, and random variations in the sphere positions.21,22
After vertical colloidal self‐assembly, thickness and struc-
Thus, the creation of defect‐free three‐dimensional (3D)
tural morphology of the resulting direct photonic crystals
photonic crystals remains still challenging, although several
were investigated by scanning electron microscopy (SEM,
reports for the production of photonic crystals by colloi-
Leo 1530). The self‐assembly defects were evaluated by
dal self‐assembly have been published. During the self‐as-
image analysis (ImageJ, 1.51p22) in a minimum of 20 SEM
sembly process, the colloidal crystal growth is affected by
images taken at lower magnification (500×). For elimina-
particle concentration, liquid evaporation rate, and the in-
tion of noise (coming from the shadowing in between the
terparticle forces in the suspension.5 As analyzed by Kuai
spheres), a Gaussian filter was applied, with no loss of infor-
et al,22 evaporation temperature and relative humidity—both
mation concerning the defects. After binarization, the area of
parameters influence the crystal growth rate by changing the
the defect was analyzed by an automated threshold definition.
evaporation rate of the solvent—have a strong influence on
Atomic layer deposition (ALD) of Al2O3 using the pre-
the film thickness, defects, and cracks. Those parameters
cursors trimethylaluminum (TMA, Sigma‐Aldrich) and de-
were also analyzed by Liu et al,5 who observed that lower-
ionized water was performed in a reactor (Savannah 100,
ing the evaporation temperature and increasing the relative
Ultratech/Cambridge Nanotech) for infiltrating the direct
humidity during the assembly process lead to the formation
photonic crystals (PS templates) at 95°C. The cycle was
of high‐quality crystals.
performed under exposure mode (0.2/60/90 seconds) with
The effect of the suspension concentration on defective
nitrogen as carrier gas (30 sccm or cm3/min). After ALD,
area is well reported in the literature. Yan et al,15 Xiao et
the polymeric template was calcined in air at 500°C for
al,1 and Weiss et al23 showed that the density of defects
30  minutes, generating the inverse opal photonic crystal
increases for higher polymer concentration. Moreover,
structure.
Zhang et al21 and Voitchovsky et al24 reached similar
The optical response of both direct and inverse opal pho-
results when studying the correlation between the type
tonic crystals was evaluated by specular reflectance mea-
of liquid used and the amount of defects. Additionally,
surements (UV‐vis‐NIR spectrometer, PerkinElmer, Lambda
Voitchovsky et al24 revealed that the density of defects
1050) from 900 to 1850 nm and at an incident angle of 8°.
can be decreased by using higher polar solvents to lower
the evaporation rate. In this paper, direct photonic crys-
tals were produced on sapphire substrates via vertical
convective self‐assembly of polystyrene particles from
3  |  RESULTS AND DISCUSSIO N
aqueous suspensions. A systematic study of self‐assembly
3.1  |  Visual characteristics
parameters, namely suspension concentration, processing
temperature, and relative humidity, was performed. The The direct photonic crystals fabricated by vertical convective
influence of these factors on the defect density and pho- self‐assembly showed an angle‐dependent reflectance behav-
tonic structure ordering was assessed by scanning electron ior when interacting with visible light, as expected. As seen
microscopy and spectroscopy techniques, respectively. in Figure 1, reflected light changes from blue‐green to red as
These results were correlated with the performance of consequence of the incident angle.25
oxide‐based inverse opal photonic crystals produced by All produced samples showed characteristic self‐assem-
controlled infiltration of the former direct photonic crys- bly stripes, which were expected from the vertical depo-
tals by atomic layer deposition. sition, as described elsewhere.3,26 The orientation of the
 |
70      CAMPOS et al.

(A) (B) F I G U R E 1   Photograph (A) and

scanning electron microscopy (SEM) image
(B) of a polystyrene (PS) direct photonic
crystal self‐assembled on a sapphire
substrate at 55°C and 70% relative humidity
(RH) using a PS suspension concentration of
1.5 mg/mL. Scale bars represent 8 mm and
2 µm, respectively

stripes is perpendicular to the growth direction of the crys- As shown in Figures 2 and 3, the thickness of the pro-
talline layer and shows periodicity. According to Yoldi et duced films increases with the suspension concentration.
al,3 the stripes are formed when the meniscus draws back Although a higher thickness is desired for a probable higher
with a discontinuous velocity, with the surface tension em- reflectance, a higher fraction of defects (line defects, point
bracing the meniscus. When the tension turns to be too ele- defects, drying cracks, stacking faults) was observed in this
vated, the film ruptures and a new meniscus starts to grow, case.
generating the stripes. The thickness dependence is in agreement with previous
work,15 which varied the total volume of the solvent. The in-
crease in the thickness by tailoring the suspension concentra-
3.2  |  Influence of suspension concentration
tion was also reported by McLachlan et al,4 for polystyrene
The polymer concentration plays an important role in the direct photonic crystals (volume variation from 1 to 5%), and
opal film growth. Liquid evaporation out of the thin menis- also by Zhang et al9; the latest work presented no quantifica-
cus leads to a constant influx, which draws the colloid into tion of the density of defects.
the area of film formation.23 The suspension concentration In the current work, the increment in the direct photonic
controls the particles flux and, consequently, the thickness of crystals’ thickness generated a higher area fraction and the
the crystal films.15 adhesion to the substrate was compromised, which was

(A) (C) (E)

(B) (D) (F)

F I G U R E 2   Top‐view and cross‐sectional scanning electron microscopy (SEM) images of polystyrene (PS) direct photonic crystals produced
at 55°C and 70% relative humidity (RH) for PS concentrations of 1 (A,B), 1.5 (C,D), and 2 mg/mL (E,F). The scale bars are equivalent to 2 µm (A,
C, E), 1 µm (B), 2 µm (D), and 3 µm (F)
CAMPOS et al.
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     71

F I G U R E 3   Effect of suspension concentration on the direct

photonic crystals’ thickness and area fraction of defects

qualitatively observed by Liu et al,27 as well. The thickness

increased from 18 to 88  µm for suspension concentrations
from 1.5 to 2.0  mg/mL, which caused an increment in the
density of defects. Supposedly, the defects were generated by
the interactions of the particles, between the free particles
still in suspension and either the substrate or the already as-
sembled layers.
In the sequence, the reflectance was measured to support
the analysis of the defects of the direct photonic crystals.
Former studies such as those of Liau et al25 and Zhou et al20
affirm that the reflectance gets lower when the amount of de-
fects increases, which was not observed in this work (Figure
4A). This behavior is most likely associated with the higher
number of assembled layers for higher suspension concen-
tration (see SEM image in Figure 2), as supported by some
authors.4,28‒30

3.3  |  Influence of temperature

Higher temperatures raise the evaporation rate during as-
sembly so that tensile stress within the films is increased.31
These tensile stresses appear during drying, in which the dis-
tance between two particles increases and cracks are formed.
Furthermore, the generation of vacancies also becomes more F I G U R E 4   Specular reflectance measurements of the polystyrene
(PS) direct photonic crystals: A, different initial concentrations (1, 1.5,
favorably generated when the evaporation rate is increased,
and 2.0 mg/mL) at 55°C and 70% relative humidity (RH); B, different
and the particles do not have sufficient time to move to the
process temperatures (40, 55, and 80°C) at initial concentration of
optimal lattice site before its deposition on the substrate.32
1.5 mg/mL, and RH at 70%; C, different RH conditions (45% and 70%)
The effect of the evaporation temperature was evaluated, at 55°C and initial concentration of 1.5 mg/mL
while the suspension concentration and the relative humidity
were kept at 1.5  mg/mL and 70%, respectively. The thick-
ness and the area fraction of defects have a clear correlation process performed at 80°C, the process time was 40% faster
with the evaporation temperature, being both increased as than those performed at 55 and 40°C. Although the amount
the temperature rises (Figure 5). It is important to point out of defects was higher for this condition (36% against 28%
that the self‐assembly process was interrupted either after for the process at 55°C), the higher thickness obtained at re-
120  hours or after total evaporation of the liquid. For the duced time could be an advantage of such high‐temperature
 |
72      CAMPOS et al.

not observed in this study. However, the samples prepared at

90°C in their work also revealed significantly more defects,
which is in good agreement with the trend observed here.

3.4  |  Relative humidity

The influence of humidity on the ordering and defects of the
direct photonic crystals can be even more critical than the
pure temperature. Relative humidity influences the evapora-
tion rate and the crystal formation.33
Figures 7 and 8 present the dependence of the film thick-
ness, amount of defects, and structural ordering. The results
showed that the higher the relative humidity (actively con-
trolled by the humidity chamber), the thicker, more ordered,
F I G U R E 5   Effect of the evaporation temperature on the film and less defective direct photonic crystals can be obtained.
thickness and area fraction of defects The samples fabricated with a 70% RH presented a higher
reflectance than those produced with 45% (Figure 4B)
self‐assembly process, if the colloidal film mechanical sta- strongly supporting the observation regarding suppressed
bility and photonic response are still considered acceptable defect at higher RH. Nevertheless, 90% RH was too high
(refer to Figure 4B). to allow the self‐assembly, so that the corresponding data
The direct photonic crystals produced at 55°C and 80°C are not available. The lack of ordering in the structure is
showed more defects such as cracks and vacancies (Figure clearly visible in the cross‐sectional analysis (Figure 8C),
6) than those fabricated at 40°C. The reflectance measure- where the samples presented a more photonic glass‐like
ments support the structural evaluation of the direct photonic appearance.35
crystals quality (Figure 4B), as the samples produced at 40°C In accordance with the observations of Kuai et al,22 no
presented higher reflectance than those fabricated at 55 and self‐assembly could be observed in case of 90% humidity;
80°C, even though the thickness was smaller (18  µm to 20 in this work, a decrease in the thickness of films was found
and 37 µm, respectively). This relationship between colloidal for values higher than 77% RH. Furthermore, Liu et al,5 pre-
films quality (direct photonic crystals in the present work) and sented similar humidity values (45, 70, and 90%) as in the
evaporation temperature has been also observed qualitatively present work and observed that the variation in RH resulted
by other authors.33,34 Chun et al,34 compared the morphology in the formation of many vacancies and dislocations, indi-
of colloidal crystals obtained at evaporation temperatures of cating that there probably exists an optimum point around
45, 60 and 70°C, with constant humidity (90%). High‐qual- 70%. Thereby, lower humidity promotes liquid evaporation,
ity crystals with respect to ordering and reflectivity were ob- increasing the evaporation rate, and bringing additional in-
tained at 45°C in 24 hours, while poorly ordered structures ternal stress, thus increasing the cracking and defects in the
(indicating many defects) were produced at the other two direct photonic crystals. At RH close to the optimum point,
temperatures, which also corroborate these results. the lateral capillary force and slower liquid evaporation result
In contrast, Im & Park26 observed that the quality of the in a better crystalline quality. Further increase in humidity
formed crystals was increased from 30 to 60°C, which was reduces the evaporation rate and too weak lateral force occur

(A) (B) (C)

F I G U R E 6   Top‐view scanning electron microscopy (SEM) images of polystyrene (PS) direct photonic crystals showing the self‐assembly
cracks according to the process temperature (40, 55, and 80°C) using PS suspensions concentration of 1.5 mg/mL, and relative humidity (RH) kept
at 70%. The scale bar represents 50 µm
CAMPOS et al.
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     73

resulting in poor crystal quality. The fact that Liu et al5 could
obtain samples, even with a low quality, might be related to
the chamber pressure used. In that case, a pressure of 6 kPa
was applied, while the current work was performed always
under atmospheric pressure.

3.5  |  Oxide‐based inverse opal

photonic crystals
After ALD and polymer template burnout, inverse opal pho-
tonic structures of Al2O3 were generated36 (insets in Figure
9). Reflectance measurements (compare them to the direct
photonic crystals in Figure 4) show a blue‐shift of the peak
position associated with a change of the photonic band gap
F I G U R E 7   Effect of relative humidity on the film thickness and (Figure 10), which is related to the different structure and to
area fraction of defects

F I G U R E 8   Top‐view and cross‐ (A) (B)

sectional scanning electron microscopy
(SEM) images of polystyrene (PS) direct
photonic crystals according to the relative
humidity (RH) of 45% (A and C) and
70% (B and D), at 55°C and PS initial
concentration of 1.5 mg/mL. In all images,
the scale bars are equivalent to 2 µm. In
the insets, the scale bars are equivalent to
0.25 µm
(C) (D)

(A) (C) (E) (G)

(B) (D) (F) (H)

F I G U R E 9   Scanning electron microscopy (SEM) images of cross section (A, C, E, and G) and top view (B, D, F, and H) of the produced
alumina inverse opals. Temperature and relative humidity were, respectively, 40°C and 45% RH (A and B); 40°C and 70% (C and D); 55°C and
70% (E and F); 80°C and 70% (G and H). Scale bars represent 5 µm in the full images and 1 µm in the insets
 |
74      CAMPOS et al.

the different refractive indexes between PS and air, or Al2O3

and air.37
Inverse opal photonic crystals present a more efficient scat-
tering system than direct photonic crystals,29,38 due to a larger re-
lationship between gap‐to‐midgap37 ratio. Since the inverse opal
photonic crystals produced in this work presented slightly lower
values for the reflectance, one can assume that an additional
small number of defects, probably vacancies, faults, and cracks
originated during polystyrene burnout were introduced. Zhang
et al39 investigated metallic inverse opals produced by solgel in-
filtration. The authors found that the defects that were already in
the photonic crystal structure were magnified and some others
were added after infiltration and burnout procedures. Zhang et
al39 found in the inverse opals some peculiar structural defects
and called them as V, P, and H defects. V defect is a pore that
is bigger than the others, P is related to deformed pores, and H
is coalesced pores. Although the used materials and the infiltra-
tion method were different from the one adopted in this work,
here some H defects were also found (Figure 11) in the produced
inverse alumina opals. The appearance of this kind of defects
and the magnification of the already existent cracks and faults
may be the cause of the reflectance suppression observed when
the data obtained before ALD and burnout are compared with
the ones accessed after these procedures. Liau et al25 and Zhou
et al20 also showed that an increase in the amount of the defect
causes a decrease in the reflectance peak. However, these papers
dealt with polymer‐based direct photonic crystals only; the use
of these as precursors for ceramic inverse opal photonic crys-
tals made by ALD is not considered. Nevertheless, a correlation
between those behaviors can be made and it can be concluded
that the majority of defects originated during the self‐assembly
step remained in the structure even after ALD. Therefore, the

F I G U R E 1 0   Specular reflectance measurements of the

polystyrene (PS) inverse opal photonic crystals for different (A) PS
suspensions initial concentration (1, 1.5, and 2.0 mg/mL) at 55°C and F I G U R E 1 1   Scanning electron microscopy (SEM) image of
70% (relative humidity [RH]); B, process temperatures (40, 55, and an inverse alumina opal photonic crystal produced with 1.5 mg/mL,
80°C) at initial concentration of 1.5 mg/mL and 70% RH; C, humidity 55°C, 70% (polystyrene [PS] concentration, evaporation temperature,
conditions (45% and 70%) at 55 °C and PS initial concentration of and relative humidity). The arrows show “H” defects.37 The scale bar
1.5 mg/mL represents 1 µm
CAMPOS et al.
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     75

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Influences of surface charge, size, and concentration of colloidal