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Busse15 AO ARSSReview
Busse15 AO ARSSReview
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United States Naval Research Laboratory
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Received 8 June 2015; revised 30 September 2015; accepted 20 October 2015; posted 20 October 2015 (Doc. ID 241841);
published 30 October 2015
We present recent advancements in structured, antireflective surfaces on optics, including crystals for high-energy
lasers as well as windows for the infrared wavelength region. These structured surfaces have been characterized
and show high transmission and laser damage thresholds, making them attractive for these applications. We also
present successful tests of windows with antireflective surfaces that were exposed to simulated harsh environments
for the application of these laser systems.
OCIS codes: (050.6624) Subwavelength structures; (160.4670) Optical materials.
http://dx.doi.org/10.1364/AO.54.00F303
Fig. 2. (a) Transmission increase of up to 91.3% for a Nd:YAG single crystal with moth eye ARSS on one surface, as compared to the
maximum theoretical value of 92%. (b) Confocal microscope and scanning electron microscope images of the moth eye surface with
scale bar 1 μm.
1.0
the transmission through the samples before and after the ARSS 0.4 rARSS-1
rARSS-2
fabrication. However, limitations on measuring low reflectance 4
0.2
with the Cary spectrometer resulted in the need for a technique
previously described [17], which uses a broadband source and 2
0.0
0.96 1.00 1.04 1.08 1.12 1.16 1.20
rARSS-2
fiber bundle to characterize very low reflection losses. Both a wavelength [µm]
405 nm Keyence confocal microscope and a scanning electron rARSS-1
microscope were utilized for characterizing the dimensional de- 0
tails of the surface structures. 0.96 1.00 1.04 1.08 1.12 1.16 1.20
wavelength [µm]
1. YAG Crystalline Materials
Typical results for the increase in transmission for Nd:YAG (a)
single crystal samples with ordered moth eye structures are
shown in Fig. 2(a), and characterizations of the surface features
are shown in Fig. 2(b). A significant increase in transmission
through a sample with ordered moth eye patterned on one
surface was measured to be 91.3%, which amounts to only
0.7% residual reflection loss from the treated surface, given
the material Fresnel loss of 8% per surface. In addition, the
crystal samples were processed with random ARSSs (rARSSs)
on one surface only, with the results shown in Fig. 3.
Remarkably, for this sample, the reflection loss was measured
to be as low as 0.08% at 1 μm.
A ceramic sample of Nd:YAG was also processed to have an
ordered moth eye surface similar to that of the crystalline sam- (b)
ple. The results for the optical transmission are shown in Fig. 4.
Fig. 3. (a) Surface reflection loss measured for random ARSSs mea-
The transmission increase of 7.5% was measured at 1.06 μm sured for one surface treated on two different single crystals of Nd:
after one surface was processed, corresponding to a maximum YAG, showing reflection losses as low as 0.08% at 1 μm (inset shows
single-surface transmission of 98.5%. the data in detail). (b) AR random surface structure features on single
In addition to the Nd:YAG crystals, ARSS fabrication was crystal Nd:YAG, as observed with confocal microscopy, where the in-
also performed on Ho:YAG, an important material for lasers set shows the details of the surface features.
F306 Vol. 54, No. 31 / November 1 2015 / Applied Optics Review
100
75
1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7
wavelength [µm]
Fig. 4. Transmission measured through ceramic Nd:YAG sample
with one side processed with moth eye surface structures similar to
those for the single crystal sample, wherein the transmission increased
by 7.5% at 1.06 μm.
Fig. 6. (a) Confocal microscope image of Ho:YAG with (b) showing
the depth of the features of approximately 670 nm and with a spacing
operating in the 2 μm wavelength region, where n 1.82. The of about 950 nm.
results for the transmission increase on Ho:YAG with a moth
eye ARSS treatment are shown in Fig. 5. From the data, we
observe that the transmission has increased to 88.6% at these structures on one side for 8–12 μm transmission, where
2 μm, which shows the reflection loss for one surface treated feature sizes are on the order of 2.2 μm spacing and 4.6 μm
with an ARSS was reduced from 8.3% to 3.2%. depth, observed using confocal microscopy and a scanning
The surface features are shown in Fig. 6(a), and were mea- electron microscope analysis.
sured using confocal microscopy analysis, with the features Figure 8 shows the long-wave IR transmission obtained for
depth and spacing shown in Fig. 6(b) observed to be approx- this sample with one side treated with the moth eye surface.
imately 670 and 950 nm, respectively. The maximum transmission in the 8–12 μm region increased
from about 48% to 63%, such that the surface transmission
2. Infrared Transmitting Windows showed an increase up to 94.6%. Additional work is in progress
The fabrication of ARSSs on spinel, an important material for to further increase the transmission over this waveband.
its UV through mid-IR transmission as well as its attractive Moth eye surfaces were also fabricated on samples of arsenic
mechanical properties, was recently reported, whereby the re- selenide, as shown by the scanning electron microscopy image
flection loss was reduced dramatically from 7% per surface to in Fig. 9. The reflectance for this one side treated on this sample
0.7% at 1 μm, and the LIDT was increased by almost a factor was reduced from 22% to 13% over the 8–12 μm region.
of 3 for windows with ARSSs compared to untreated windows However, since this glass, like other sulfur- and selenide-
[17]. AR moth eye structures on sapphire, a comparable containing chalcogenide glasses, has a low temperature
window material, have also been reported with excellent softening point (<200°C), the AR performance may be greatly
performance [22]. improved by instead using the method we have already dem-
We have recently characterized moth eye structures fabricated onstrated for imprinting the moth eye AR surfaces on the sur-
on germanium windows, which are important for mid- to long- faces. In that work, a significant reduction in the reflectance
wave IR transmission. Figure 7 shows a sample fabricated with from 17% to 3% was measured for the moth eye imprinted
end faces of arsenic sulfide fibers [18].
100
B. Laser-Induced Damage Threshold Results
96
The LIDT for a high-power laser incident on a surface with
bulk transmission [%]
theoretical maximum
92 scratches or defects is normally much lower than that for an
optic with a highly polished, smooth surface [23]. Similarly,
88 ARSS one might expect the surface of an optic with moth eye features
84 untreated to be more susceptible to laser damage. However, in a recent
80
study, modeling was carried out for the effects of the electro-
magnetic field impinging on such a surface, and showed that
76 there is no enhancement of the field intensity at the peaks of the
72
moth eye structures, as might intuitively have been expected
1.8 1.9 2.0 2.1 2.2 2.3 2.4 [24]. To our knowledge, this is the first theoretical study that
wavelength [µm] lends support to the experimentally observed high LIDT for
Fig. 5. Transmission measured through crystalline Ho:YAG with surfaces with ARSSs.
one side processed with moth eye ARSS, wherein the transmission in- We conducted laser damage testing on the laser crystals fab-
creased to 88.6% at 2 μm. ricated with the moth eye features and compared the results to
Review Vol. 54, No. 31 / November 1 2015 / Applied Optics F307
Fig. 7. Germanium window with moth eye surface and expanded view using confocal microscopy analysis. Scale bar 10 μm in confocal image
on the right.
the results for the untreated samples. These tests were con- duced damage thresholds for the surfaces with moth eye treat-
ducted by Spica Technologies, Inc. using standardized tech- ments are very similar to those obtained for the untreated
niques with sources at 1.064 and 2.055 μm. The laser at surfaces. Although these damage thresholds are relatively low
1.064 μm used for the Nd:YAG samples had the following when compared to those reported for other YAG materials [22],
parameters: linear polarization, incidence angle 0°, TEM00 we believe this was due to surface defects in the sample caused
beam profile, 10 ns pulse width (full width at half-maximum), by the polishing process on the samples used for this study.
300 μm diameter spot size (at 1 · e−2 ), and a 20 Hz repetition Figure 11 shows results for the Ho:YAG crystalline samples
rate. The laser damage testing consisted of 200 shots per site with AR surface structures, compared to that with an AR coat-
over a total of 90–100 sites on each sample. The laser used at ing (HoYAG-ARC) and the untreated sample. The LIDT for
2.055 μm for Ho:YAG was characterized by the following the sample with ARSSs was much lower than that for both the
parameters: linear polarization, incidence angle 0°, TEM00 AR-coated sample as well as the untreated sample. The reasons
beam profile, 35 ns pulse (full width at half-maximum), 88 μm for this discrepancy are the subject of further analysis.
diameter spot size (at 1 · e−2 ), and a 400 Hz repetition rate. For
these tests, 4000 shots per site were used, with a total of 80–
100 sites per sample. The onset of damage was defined to occur 4. ENVIRONMENTAL TESTING AND ANALYSIS
when it could be visibly observed with a 150× Nomarski dark-
Although it was shown previously that optics with ARSSs that
field microscope or when a laser-induced plasma or increased
were intentionally contaminated can then be successfully
scatter was detected using a helium–neon laser.
cleaned with conventional methods [17], a major concern has
Figure 10 shows the results obtained for (a) the Nd:YAG
been whether optics with ARSSs can be used in real environ-
single-crystal samples and (b) the Nd:YAG ceramic samples,
ments. Military systems such as those using silica glass output
where the moth eye-treated sample results are compared to
windows as exit apertures for high-energy lasers will operate on
those without surface treatment. In both cases, the laser-in-
a variety of land, sea, and airborne platforms. Therefore, we
investigated the performance of silica windows with random
AR surface structures by testing the optical transmission before
Fig. 8. Transmission of germanium sample before (orange curve) Fig. 9. Scanning electron microscopy image of an arsenic selenide
and after (red curve) the fabrication of moth eye surface structures glass sample with moth eye surface features optimized for 8–12 μm
on one side. transmission.
F308 Vol. 54, No. 31 / November 1 2015 / Applied Optics Review
40 untreated 40
-2 untreated
LDT: 4.9 J.cm -2
LDT: 4.3 J.cm
20 20
0 0
0 2 4 6 8 10 0 2 4 6 8 10
-2 -2
(a) fluence [J.cm ] (b) fluence [J.cm ]
Fig. 10. Laser-induced damage thresholds measured at 1064 nm for (a) Nd:YAG single crystal samples with and without moth eye on one surface
and (b) Nd:YAG ceramic samples also with and without moth eye on one surface.
and after exposure to simulated environments of sea-based and applied, where “FS” corresponds to the untreated fused silica
land-based systems. samples and “ARSS” refers the sample with the random AR
Fused silica glass samples (1 0 0 diameter discs or squares) with surface structures. The samples’ transmission before the test
random ARSSs were prepared by using conventional reactive (FS-1 and ARSS-1) showed the typical transmission as previ-
ion etching techniques with the appropriate reactive gases to ously reported [17], whereby there is some reduction due to the
create random AR surface structures on the surface with a maxi- diffraction at the shorter wavelengths in the ARSS sample.
mum transmission near 1 μm. The measured transmission of However, the transmission is above 95% in the 1 μm wave-
>95% for a sample with one surface treated was within the length region for the sample with ARSS, as was the desired
experimental error of the maximum theoretical transmission of performance. If needed, tailoring the ARSS fabrication will give
96.5%. In addition, samples of fused silica without any AR higher visible transmission for the samples.
surface treatment were used as controls in all the tests. The As shown in Fig. 12, the curves for FS-2 and ARSS-2 are
transmission was measured before and after the samples were the transmission results after exposure to the dried seawater,
subjected to the environmental conditions. Following the tests, showing the dramatic reduction at all wavelengths. Following
the samples were cleaned and the transmission was re-measured those measurements, the samples were cleaned with a stream of
to determine if there was any change observed from the original deionized water and dried with dry nitrogen gas. Remarkably,
results. the transmission of the cleaned samples for both the fused silica
(FS-3) and the sample with ARSS (ARSS-3) both returned to
A. Seawater Contamination Tests the original values. The transmission results overlapped com-
The samples of fused silica with and without ARSSs were ex- pletely with the curves for FS-1 and ARSS-1 on the plot, so
posed to Key West seawater by using a syringe to deposit a they are not distinguishable. These results demonstrate that
0.4 ml drop onto each sample, then allowing the water to dry there were no residual problems with contamination due to
completely on the samples in air. Figure 12 shows the results for
the tests of transmission before and after the seawater was
-2
0.6 1.7 2.9 [GW.cm ]
6
HoYAG-ARSS
number of damaged sites
-2
LDT = 25 J.cm HoYAG-ARC
5 -2
LDT = 78 J.cm
HoYAG
1 (uncoated)
-2
LDT > 100 J.cm
0
0 20 40 60 80 100 120
-2
pulse energy [J.cm ] Fig. 12. Transmission of fused silica (FS) and silica with ARSS
Fig. 11. Summary of the laser-induced damage threshold measure- (ARSS) before and after seawater contamination, where 1, 2, and 3
ments for crystalline Ho:YAG (red: with ARSS; blue: with AR coating; are the labels for the samples before seawater application, with dried
and green: uncoated). seawater, and after cleaning with deionized water, respectively.
Review Vol. 54, No. 31 / November 1 2015 / Applied Optics F309
the salt or water on the samples with ARSS, thus showing their transmission for ARSS-3 in the infrared (at wavelengths above
utility for systems in a marine environment. 1 μm) was measured to be within 1% of that before exposure
(ARSS-1), and notably, there was no increase in the OH ab-
B. High Temperature and Humidity Environmental sorption of the sample. However, at wavelengths below 1 μm,
Tests
there was a slight reduction (<5%) in transmission from the
The Tropical High Bay facilities at the Naval Research original values, possibly due to residual dirt that was not
Laboratory in the Naval Autonomous Systems Laboratory were removed from the surface.
utilized for these tests, whereby conditions are maintained at
80°F and 80% relative humidity so as to simulate a southeast
Asian jungle environment, complete with native plants and a 5. SUMMARY
stream of running water [25]. The temperature and humidity We have obtained results for crystalline laser optics and infrared
were monitored and stayed within these parameters during the windows that demonstrate the excellent optical performance
test run on the fused silica samples with and without ARSSs. of AR surface structures etched directly into the optics.
The samples were attached to a platform on a catwalk 15 feet These features serve the same purpose as a low-reflectance AR
above the floor of the laboratory, with intention to leave them coating, but without the less-desirable properties, such as coat-
there for 48 h exposure. Care was taken to put the samples on ings delamination or low laser-induced damage thresholds.
standoffs inside a dish with holes drilled in it to preclude stand- Crystalline samples of Nd:YAG and Ho:YAG with AR surface
ing water accumulation. features showed reflectances as low as 0.08% and LIDTs in
However, after one day, it was discovered that the sample the near-infrared that were comparable to the untreated or
holder mounting had come loose when a fan that circulates AR-coated samples that were tested. The results for long-wave
air in the room came on automatically, and the samples had IR transmission in the 8–12 μm region showed good perfor-
fallen into the dirt on the lab floor below. The (now dirty) sam- mance for both the germanium and arsenic selenide glass
ples were moved back into the tray, which was attached more samples. Finally, the utility of AR surface structures in real envi-
securely, then left for the remainder of the 48-h period. Thus, ronments was tested on silica glass samples with random ARSSs
this test also led to the evaluation of methods to clean dirt from that were exposed to either seawater contamination or two
the samples. days in a tropical environment. The samples that were exposed
Figure 13 shows the transmission results for the samples and then cleaned using the typical methods showed that the
with labeling as used before, whereby 1 corresponds to trans- infrared transmission returned to previous levels. For the sam-
mission of the samples before testing, label 2 is for samples after ples exposed to dirt contamination in the tropical environment,
exposure, including the dirt, and label 3 is for cleaned samples. only a small change in transmission was observed at visible
After exposure, the samples were cleaned by rinsing them wavelengths, and was most likely due to residual contaminants
with deionized water and wiping them with a lint-free, soft on the surface.
cloth soaked in isopropyl alcohol. For the fused silica sample, These results demonstrate the utility of ARSSs on laser
the transmission returned to the original levels (comparing optics, as well as infrared and visible-transmitting windows for
FS-1 and FS-3). For the ARSS sample, the transmission for laser systems and other applications. The silica windows with
ARSS-2 was not as low as that for the untreated fused ARSSs not only perform well optically, but also show promise
silica (FS-2) after the high bay exposure. After cleaning, the for being operational in the field for high-energy laser systems,
whether it be a land- or sea-based environment.
REFERENCES
1. M. J. Minot, “Single-layer, gradient refractive index antireflection films
effective from 0.35 to 2.5 μm,” J. Opt. Soc. Am. 66, 515–519 (1976).
2. T. A. Hansen, C. Johnson, Jr., and R. R. Wilbarg, “Method for fabri-
cating non-reflective semiconductor surfaces by anisotropic reactive
ion etching,” U.S. patent 4,229,233 (21 October 1980).
3. L. M. Cook, W. H. Lowdermilk, D. Milam, and J. E. Swain,
“Antireflective surfaces for high-energy laser optics formed by neutral
solution processing,” Appl. Opt. 21, 1482–1485 (1982).
4. L. M. Cook, S. Ciolek, and K. H. Mader, “Integral antireflective surface
production on optical glass,” J. Am. Ceram. Soc. 65, C-152–C-155
(1982).
Fig. 13. Samples transmission of fused silica (FS) and silica with 5. T. Lohmueller, R. Brunner, and J. P. Spatz, “Improved properties
ARSS before and after exposure in the Tropical High Bay and after of optical surfaces by following the example of the ‘Moth Eye’,” in
cleaning. Residual dirt on the sample of ARSS-3 caused some reduc- Biomimetics Learning From Nature, A. Mukherjee, ed. (Intech, 2010),
tion in visible transmission, but not in the infrared. Chap. 22.
F310 Vol. 54, No. 31 / November 1 2015 / Applied Optics Review
6. D. S. Hobbs, B. D. MacLeod, and E. Sabatino III, “Continued advance- 17. L. E. Busse, C. M. Florea, J. A. Frantz, L. B. Shaw, I. D. Aggarwal,
ment of laser damage resistant optically functional microstructures,” M. K. Poutous, R. Joshi, and J. S. Sanghera, “Anti-reflective surface
Proc. SPIE 8530, 85300O (2012). structures for spinel ceramics and fused silica windows, lenses and
7. T. Maier, D. Bach, P. Müllner, R. Hainberger, and H. Brückl, optical fibers,” Opt. Mater. Express 4, 2504–2515 (2014).
“Antireflective surface structures in glass by self-assembly of SiO2 18. J. Sanghera, C. Florea, L. Busse, B. Shaw, F. Miklos, and I. Aggarwal,
nanoparticles and wet etching,” Opt. Exp. 21, 20254–20259 (2013). “Reduced Fresnel losses in chalcogenide fibers by using anti-
8. K. J. Major, C. M. Florea, M. K. Poutous, L. E. Busse, J. S. Sanghera, reflective surface structures on fiber end faces,” Opt. Express 18,
and I. D. Aggarwal, “Surface transmission enhancement of ZnS via 26760–26768 (2010).
continuous-wave laser microstructuring,” Proc. SPIE 8968, 896810 19. “Anti-reflective plastics inspired by moths’ eyes,” The Agency for
(2014). Science, Technology and Research (A*STAR), ScienceDaily, 24
9. C. G. Bernhard and W. H. Miller, “A corneal nipple pattern in insect May 2012. www.sciencedaily.com/releases/2012/05/120524134520
compound eyes,” Acta Physiol. Scand. 56, 385–386 (1962). .htm.
10. W. H. Southwell, “Gradient-index antireflection coatings,” Opt. Lett. 8, 20. G. Villalobos, S. Bayya, W. Kim, J. Sanghera, B. Sadowski, R. Miklos,
584–586 (1983). C. Florea, and I. Aggarwal, “Polished spinel directly from the hot
11. W. H. Southwell, “Pyramid-array surface-relief structures producing press,” in Advances in Ceramic Armor VIII, J. J. Swab, M. Halbig,
antireflection index matching on optical surfaces,” J. Opt. Soc. Am. and S. Mathur, eds. (Wiley, 2012).
A 8, 549–553 (1991). 21. Q. Chen, G. Hubbard, P. A. Shields, C. Liu, D. W. E. Allsopp, W. N.
12. J. J. Cowan, “Aztec surface-relief volume diffractive structure,” J. Opt. Wang, and S. Abbott, “Broadband moth-eye antireflection coatings
Soc. Am. A 7, 1529–1544 (1990). fabricated by low-cost nanoimprinting,” Appl. Phys. Lett. 94, 263118
13. P. Lalanne and D. Lemercier-Lalanne, “On the effective medium (2009).
theory of subwavelength periodic structures,” J. Mod. Opt. 43, 22. D. S. Hobbs, B. D. MacLeod, E. Sabatino, T. M. Hartnett, and R. L.
2063–2085 (1996). Gentilman, “Laser damage resistant anti-reflection microstructures in
14. Y. Kanamori, H. Kikuta, and K. Hane, “Broadband antireflection Raytheon ceramic YAG, sapphire, ALON, and quartz,” Proc. SPIE
gratings for glass substrates fabricated by fast atom beam etching,” 8016, 801628 (2011).
Jpn. J. Appl. Phys. 39, L735–L737 (2000). 23. R. M. Wood, Laser-Induced Damage of Optical Materials (Institute of
15. C. Aydin, A. Zaslavsky, G. J. Sonek, and J. Goldstein, “Reduction of Physics, 2003), Chap. 5.
reflection losses in ZnGeP2 using motheye antireflection surface relief 24. R. J. Weiblen, C. R. Menyuk, C. Florea, L. Busse, B. Shaw, I.
structures,” Appl. Phys. Lett. 80, 2242–2244 (2002). Aggarwal, and J. Sanghera, “Irradiance enhancement and increased
16. D. S. Hobbs, B. D. MacLeod, and J. R. Riccobono, “Design, fabrica- laser damage threshold in As2S3 motheye antireflective structures,”
tion, and measured performance of anti-reflecting surface textures in Opt. Lett. 40, 4799–4802 (2015).
infrared transmitting materials,” Proc. SPIE 5786, 40–57 (2005). 25. www.nrl.navy.mil/research/automomus‑systems.