Laser damage resistant anti-reflection microstructures

in Raytheon ceramic YAG, sapphire, ALON , and quartz.

TM

Douglas S. Hobbs*, Bruce D. MacLeod, Ernest Sabatino III

TelAztec LLC, 15 A Street, Burlington, MA, USA 01803-3404

Thomas M. Hartnett^, Richard L. Gentilman

Raytheon Integrated Defense Systems, Mechanical Engineering Directorate
350 Lowell Street Street, Andover, MA, USA 01810

ABSTRACT
A study of the laser induced damage threshold (LiDT) of anti-reflection (AR) microstructures (ARMs) built in the end
facets of metal ion doped yttrium aluminum garnet (YAG) laser gain material, has been conducted. Test samples of
undoped and ytterbium-doped polycrystalline YAG produced by Raytheon Company were processed with ARMs in one
surface and subjected to standardized pulsed LiDT testing at the near-infrared (NIR) wavelength of 1064nm. As
received YAG samples with a simple commercial polish were also submitted to the damage tests for comparison, along
with YAG samples that were treated with a single layer thin-film AR coating designed for maximum transmission at
TM
1064nm. Additional samples of single crystal sapphire and quartz, and polycrystalline ALON windows were prepared
with thin-film AR coatings and ARMs textures to expand the 1064nm laser damage testing to other important NIR
transmitting materials. It was found that the pulsed laser damage resistance of ARMs textured ceramic YAG windows
is 11 J/cm2, a value that is 43% higher than untreated ceramic YAG windows, suggesting that ARMs fabrication
removed residual sub-surface damage, a factor that has been shown to be important for increasing the damage resistance
of an optic. This conclusion is also supported by the high damage threshold values found with the single layer AR
coatings on ceramic YAG where the coatings may have shielded the sub-surface polishing damage. Testing results for
the highly polished sapphire windows also support the notion that better surface preparation produces higher damage
resistance. The damage threshold for untreated sapphire windows exceeded 32 J/cm2 for one sample with an average of
27.5 J/cm2 for the two samples tested. The ARMs-treated sapphire windows had similar damage thresholds as the
untreated material, averaging 24.9 J/cm2, a value 1.5 to 2 times higher than the damage threshold of the thin film AR
coated sapphire windows.
Keywords: Antireflection, AR, Motheye, Microstructures, LIDT, YAG, High Power Lasers, Thin-Film AR Coatings

1. INTRODUCTION
Metal ion doped yttrium aluminum garnet (YAG) material is widely used as a gain medium in high power solid-state
lasers[1,2]. Increasingly, the wide transmission bandwidth and mechanical durability of polycrystalline YAG has made
its use as an infrared transparency attractive for laser targeting and sensor applications[3-7]. Raytheon has been
developing ceramic YAG material to address the need for large area materials with lower costs than those that can be
produced with conventional single crystal growth processes. Ceramic YAG can be produced with a greater refractive
index uniformity than single crystal YAG, and can be doped in a more flexible manner to yield higher dopant
concentrations or spatially varied concentrations. As solid state laser gain media becomes larger in order to scale to
higher power levels, these factors will become increasingly significant.

To add optical functions such as wavelength filtering, polarization, or anti-reflection (AR) to YAG laser rods or
windows currently requires the deposition of multiple layers of dissimilar thin-film materials designed to produce
interference effects for light within a target wavelength band. However, these thin-film material stacks are easily
damaged at laser power levels that severely limit the lifetime, output power, and reliability of a laser system. Surface
relief microstructures offer an alternative to thin-film coatings for high power laser systems[9]. In standardized pulsed
laser damage testing at multiple wavelengths ranging from the near UV through the long wave infrared, AR
microstructures (ARMs) built in the surface of many types of materials have consistently exhibited damage thresholds 2
to 5 times higher than thin-film AR coatings[10]. For this work, the laser damage resistance of ARMs textures built in
TM
Raytheon ceramic YAG, Crystal Systems single crystal sapphire, Surmet poly-crystal ALON , and single crystal quartz

*
dshobbs@telaztec.com; phone 1 781 229-9905; fax 1 781 229-2195; www.telaztec.com
^
thomas_m_hartnett@raytheon.com; phone 1 978 470 9302; fax 1 978 470 9003

Window and Dome Technologies and Materials XII, edited by Randal W. Tustison, Proc. of SPIE
Vol. 8016, 80160T · © 2011 SPIE · CCC code: 0277-786X/11/$18 · doi: 10.1117/12.883272

Proc. of SPIE Vol. 8016 80160T-1

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 windows was compared to the damage resistance of untreated and thin-film AR coated windows using a standardized
testing service provided by Quantel USA. The tests were run at a near-infrared (NIR) wavelength of 1064nm where the
use of ARMs technology has the potential to significantly increase the damage threshold of pump beam integrators, gain
media facets, and laser cavity components.

2. ARMs TEXTURE DESIGN MODELING

Forming ARMs textures out of the same material as a bulk optic or window eliminates the power handling and
bandwidth limitations caused by the need for planar interfaces and dissimilar materials when applying conventional
thin-film AR coating technology. Because both surface relief textures provide a gradual change in the refractive index
at a material boundary, light can propagate through the boundary without material damage at energy levels that are
much higher than that found with thin-film interference coatings. Multiple types of ARMs textures, commonly known
as Motheye textures in the literature,[11-14] have been demonstrated to outperform AR coatings in overall light reflection
suppression, operational bandwidth, field of view, polarization, environmental durability, radiation resistance, long term
reliability, and power handling capacity[15-19]. For YAG laser applications the power handling capacity of ARMs
technology is the main focus. Figure 1 illustrates three types of ARMs textures that can be fabricated in the end facets
of a YAG laser rod to eliminate reflections over the NIR wavelength range where most metal ion dopants such as
neodymium, erbium, and ytterbium produce laser emission. The features in the ARMs texture are organized in a
periodic array with a spacing that is much smaller than the target wavelength to ensure that there will be no transmission
loss due to diffraction. For normal incidence illumination with 1064nm wavelength light of an ARMs texture in YAG,
the array spacing
, must be set less than 1064/1.82 =585nm (/n, where n is the refractive index of YAG at a
wavelength =1064nm), to avoid diffraction. The height h of the features in the array impacts the performance
bandwidth with taller structures typically operating over a wider spectral range. Feature shape is most significant for
the ARMs fabrication process where lower aspect ratio, flat top profile structures can be made more uniform over larger
areas in a wider range of materials. [A fourth diagram depicting a single layer thin-film AR coating is also shown in
Figure 1 where the coating thickness is designed to be the target wavelength divided by four times the coating refractive
index. Maximum performance is obtained when the coating refractive index matches the square root of the bulk optic
refractive index].

AOI=0°

h

PYRAMIDS
HYBRID
POST/HOLE
THIN FILM

Figure 1: Diagrams representing three types of ARMs textures and a single layer AR coating.

For the YAG laser application, a more detailed prediction of the performance of the various types of ARMs textures
was made through optical modeling. A three-dimensional computer model was constructed using a vector diffraction
program based on rigorous coupled wave theory that solves Maxwell’s equations at each layer in a stepwise
approximation. Up to nine two-dimensional layers were employed to accurately model arrays of three-dimensional
structures similar to those depicted in Figure 1. The library includes published data for the refractive index of YAG to
properly account for dispersion. Figure 2 gives the simulation results where the predicted transmission of normally
incident NIR light propagating from an air environment through the ARMs texture and into the bulk YAG material is
plotted over the spectral range of from 0.9
m to 1.9
m. Cross sectional diagrams showing the dimensions for each
design variant are inset in the plot. An array spacing of 500nm was set for all variants where no diffraction is possible
for wavelengths longer than 905nm (this includes the pump band for ytterbium-doped YAG which is relatively wide
spanning the range of from 930-960nm as can be seen in Figure 3 below).

Broad-band transmission is predicted for Motheye-type ARMs textures consisting of arrays of both linear profile (solid
black curve) and sinusoidal profile (solid grey curve) pyramids. The tip of each square based cone structure is removed
in the simulation to better match the structures that are typically fabricated. Notice that the height of the sinusoidal cone
structures is just 80% of the height needed to attain nearly equivalent performance from linear profile structures. This

Proc. of SPIE Vol. 8016 80160T-2

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 dependence on cross sectional profile becomes increasingly important for higher refractive index materials such as
silicon and germanium[9,17], and for wider bandwidth applications where higher aspect ratio structures are needed.
SWS-type ARMs textures consisting of an array of square profile mesas (dotted black curve), produce maximum
transmission at the target design wavelength of 1030nm, but falls off more rapidly at longer wavelengths. Binary
profiles perform in a manner that is equivalent to a single layer thin-film AR coating, but with the important design
advantage that low reflectance can be created for materials such as fused silica or quartz where thin-film materials with
the needed low refractive index (~1.2) are fragile (sol-gel) or do not exist. Hybrid ARMs textures consisting of an array
of tapered posts (dashed grey curve), provide good performance at the target wavelength that decreases only slightly at

'
longer wavelengths. With an aspect ratio just 50% higher than SWS mesas, and only 60% of the pyramid structure
aspect ratio, Hybrid textures offer a good balance between ease of fabrication and performance.

100
1 00 .-----.z-n
Diffraction Edge 905nm

-r . tZ-- Motheye
Motheye
100
Predicted Infrared Transmission, %

a? T-Pyramids
C
99
99
1
. '.._.. 500h r-sinusois
T-Sinusoids
4h
400h
- 99

0
° 98
98 Yb:YAG
Yb:YAG Predicted Transmission of NIR Light 98

laser X

laser Propagating From Air Through ARMs -
4 Into
Into YAG,
YAG, 500nm
500nm Pitch,
Pitch, AOI=0°
AOl=0' HYBRID
97 1030nm
lO3Onm 300h 97
ii
-
i 96
96 II SWS POSTS -
SWS POSTS 96
/i 200h
0
=0.50

A=0.50
. 95
95 95
(5
.4-
ii 05
0.5
I ' I--f'
I
I 04
0.4

9494
.E 94
94 Yb:YAG
Yb:YAG
#0.3%
I
0.3

' II 0.2

0.2
pump
.1 3 L_J I

93 940nm PYRAMIDS

PYRAMIDS SINUSOIDS

SINUSOIDS HYBRID

HYBRID POST/HOLE

POST/HOLE 93

92 YAG 92

Single
Single Surface
Surface -
91
91 91
0.90
0.90 1.0
1.0 1.1
1.1 1.2 1.3
1.3 1.4
1.4 1.5 1.6 1.7
1.7 1.8 1.9
19
Wavelength, pm
μm
Figure 2: Predicted single surface transmission through various design ARMs textures in YAG.

3. ARMs TEXTURE FABRICATION AND MEASURED PERFORMANCE

Raytheon provided 18 samples of their ceramic YAG material doped with ytterbium, and 10 samples of their un-doped
ceramic YAG. Each sample was cut and polished by Raytheon to a size of 10x10mm, 1.8 or 2.0mm thick. The
transmission and reflection of each sample was measured using a grating-based NIR spectrometer operating over the
wavelength range of 0.9
m to 1.7
m. Two multi-mode fiber optic cables equipped with collimating lenses were used
to transmit a broad-band light source through each sample, and to return the transmitted light to the spectrometer input.
A single bifurcated fiber cable was used to send and receive the broad-band light source during reflectance
measurements. Transmission measurements of the YAG samples were also made in the mid-infrared wavelength range
of from 1.8
m to 20
m using a Nicolet 550 FTIR spectrometer. Figure 3 shows the transmission data where the low
dispersion of Yb:YAG (solid grey curve) and un-doped YAG (dashed black curve) leads to a relatively flat transmission
– 83% to 84% - over the spectral range from 1
m to 4
m. Note the ytterbium absorption band centered at 0.94
m.
The transmission curve represents the average of all the samples received where the transmission variation part to part
was less than the measurement system error of 0.5%.

ARMs textures of the Figure 2 design are created using the two-stage lithography and etch
process illustrated in Figure 4. The process begins with the patterning of an etch mask in a
sacrificial material coated or deposited on the surface of the window (steps 1 thru 4), and is
followed by a dry plasma etch process to transfer the mask pattern directly into the window
material (steps 5 thru 7). A laser based, maskless, non-contact, large area interference
lithography[20] (IL) system like the one depicted in the image on the right, was configured to
generate a honeycomb array of holes or posts with a periodicity of 525nm in a photosensitive
layer coated on the surface of each YAG window (steps 3 and 4).

Proc. of SPIE Vol. 8016 80160T-3

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 90
090
Measured Transmission, %

80
80

70-
70
I
NIR:
NIR: 0.85
0.85-- 1.7Opm
1.70 μm

-.
FTIR,: 1.72 - 22 μm
1iiWk#fl-vi I a 90

80

70
E -
60
2 60- 60
I RAYTHEON
RAYTHEON Ceramic YAG
Ceramic YAG
50 Y01-Y18UT,Yb:YAG,1.8mm
YOl Y18UT,Yb:YAG,1.8mm
50
Yb

Yb Y20-Y29UT,YAG,2.0mm
Y20-Y29UT.YAG2.Omm
40
40 Absorption

Absorption 40
m Band

Band 10x10 mm
lOxlO mm
30-
30 30
5
20
20 20
0.90
0.90 1.0
1.0 2.0
2.0 3.0
3,0 4.0 5.0 6.0
Log Wavelength,
Log Wavelength, pm
μm
Figure 3: Measured IR transmission of 1.8 and 2.0mm thick Raytheon ceramic YAG windows prior to ARMs fabrication.

1

2

Substrate Clean
Substrate Clean

t_tin
I''
-

I
'Ti,
I!
S ''
' '' I
,
I
'
Ti
I
g

I
'_I
'
'' '
'II
Ti
I I

I
I'I' ''.r-i' IS '-i
I
IS
,
I
¶
,'
' S
S
I

2 Spin Coat Photoresist

Photoresist 3

3\ Interference Lithography

Ii,terterei-erterence Lithography 4

4 Resist Wet Development
Development

'V vVV
=1
V. V

V p-
V;vL
5
LOption: Deposit
5 / LiftoffHard
Deposit/Liftof HardMask
Mask

6
DRY ETCH (RIE or IBM)
7
Strip: Metal
Strip: Metal // Resist
Resist Mask
Mask

Figure 4: Process flow diagram for the fabrication of ARMs textures in a window or optic surface.

Etching microstructures in the surface of such a mechanical durable and chemically resistant material as YAG is a
major challenge. A wide search of the literature did not produce any potential plasma etch chemistries for yttrium
aluminum garnet, in fact only references to the etching of yttrium oxide and aluminum oxide thin-films could be
found[21-23]. To verify the assumption that a simple physical etch process based on ion bombardment would not be
practical, one YAG sample was patterned with a photoresist mask as described above and etched by argon ion milling.
The milling rate for YAG was found to be less than 3nm/min which would require between 100 and 200 minutes of
milling through a similarly low milling rate etch mask material such as silicon oxide. The alternative was to use an in-
house inductively coupled plasma (ICP) reactive ion etch (RIE) system that has been capable of etching sapphire and
ALON ARMs textures at rates up to 45nm/min. The fluorine based gases and high plasma energies used in the sapphire
RIE/ICP processes remove photoresist at a very high rate, and therefore the typical photoresist etch masks defined by
the IL process must be converted to a more durable material such as titanium or nickel. Figure 5 shows scanning
electron microscope (SEM) images of the typical hole pattern created by the IL process as an intermediate step in the
process of defining a hard metal etch mask (step 5 in Figure 4). The metal required is deposited by evaporation or
sputtering methods over the photoresist pattern and onto the YAG substrate that is exposed at the bottom of each hole.
A wet chemical liftoff process is then used to rapidly dissolve the photoresist and lift off the metal layer that was
deposited on top of the resist – leaving an array of metal pads like those shown in the SEM image of Figure 6.

Proc. of SPIE Vol. 8016 80160T-4

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 Resist
Resist

1;
-w
.

Yb:YAG

Y02, resist 70°

70 1.Opm 23000X Y02. resist 0°
1.Opm 25000X Y02, resist 90°

90 I .Opm 25000X
Figure 5: Elevation (70°), overhead (0°), and profile (90°) SEMs of an ARMs patterned resist mask layer on a YAG crystal.

METAL MASK ON SAPPHIRE 70°

7Q
1.00 urn 20000 X fl 0°

.eS
Figure 6: Elevation (70°), and overhead (0°) SEMs of an ARMs patterned metal mask layer on a sapphire window.
1.00 pm 20000X I

After metallization, an exhaustive series of etch trials were conducted using the seven fluorine and bromine based gases
available in the RIE/ICP tool, and beginning with the successful parameter set used for defining ARMs textures in
sapphire and ALON. These trials met with little to no success producing only physical ablation of the YAG material at
rates similar to ion milling, indicating that the chemical bonds in yttrium aluminum garnet were much harder to break
than the aluminum oxide bonds in sapphire. With such low chemical activity, the composition and thickness of the
metal hard mask became critical. After several cycles of metal deposition, etching, stripping, and re-work, an etch
process based on maximizing the ICP power and minimizing the chamber pressure yielded etch rates for YAG that were
in the 10 to 15nm/min range with comparable metal mask ablation rates. These rates and mask-to-YAG etch selectivity
were sufficient to generate the binary SWS-type ARMs textures as well as the tapered mesa HYBRID-type ARMs
textures. Figure 8 shows SEM images of the SWS-type ARMs texture etched in the surface of an un-doped YAG
sample used for process development. Further process optimization is expected to yield the cone structures needed for
improved wide bandwidth performance.

;t )000000000C
N' 000000000r pS a a.
t'P'00000000CC
2000 0000oo
00C)0O000OC
flflrfltW%rrsd
him
70°
I Y20A 0°
I I
88°

Figure 7: Elevation (70°), overhead (0°), and profile (90°) SEMs of ARMs etched in the surface of a Raytheon YAG crystal.

The performance attained with these first YAG ARMs textures was established with reflection and transmission
measurements made with the NIR grating based spectrometer described above. Figure 8 is a plot showing the
transmission of the samples submitted to the pulsed laser damage testing where the data has been normalized by
referencing each trace to the single surface transmission established by the optical material constants given in the
literature[8]. Measurements for the untreated YAG windows are relatively flat over the 1.1 to 1.7
m range and
normalized at 91-91.5%. Two Yb-doped YAG windows processed with ARMs textures and labeled Y13ME and
Y11ME, are represented by the black dashed and dotted curves in the figure respectively. An un-doped ARMs-textured
window Y26ME is shown as the solid grey curve in the figure notable due to the lack of short wave transmission loss
caused by the Yb absorption present in the doped samples. The ARMs textured samples show a modest transmission
increase over the untreated windows due to the limited etch depth attained with the process as described above – a
problem which will be resolved with future etch process development work.

Proc. of SPIE Vol. 8016 80160T-5

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 Two additional Yb-doped YAG windows were sent to a thin-film AR coating service provided by Quality Thin Films,
Inc. of Oldsmar Florida (QTF). QTF applied their proprietary high damage threshold single layer AR coating by ion
beam assisted deposition, targeting maximum transmission at 1064nm. The coating performs well with less than 0.3%
reflectance measured at the target wavelength and a 0.1% minimum reflection measured at 1030nm. In transmission the
thin film coated Yb-doped YAG windows labeled Y16TF and Y18TF and represented by the solid black curve in Figure
8, show a value of just under 99% at 1064nm due to the roll off in the proximity of the Yb absorption band.

-100
100 100
100
(Normalized)

- 99 -I
1064nm
1064nm
Y16TF --ARC
Y1GTF ARC
99
99
98-
98 Y13ME
Y13ME --ARMs
ARMs 98
98

97
- Y26ME
Y2GME 97
97
ARMs
ARMs -
Measured Transmission, %

96
96 96

95 -- = \-
95 Diffraction
Loss
I..- -

J':
95

I 94 94

£93
C 92
\I 93
92
Yb
Yb
Absorption
Edge
YAG - Yb:doped
Y11ME
Y11ME --ARMs
ARMs
93
93
92
92
UNTREATED
UN
91

..87
91 91
Ttnrm,V1618_TF
T%nrm,Y1618_TF -
90
A
T%nrm,V13_ME
T%nrm, Y13_ME
Tt
T%nrm,,V26_ME
Y26_ME -
90
90
89 YAG--Undoped
YAG Undoped r%nrm,yl1_ME
T%nrm, Y11_ME 89
89
Tt nrm, Vb:YAG
T%nrm, UT
Yb:YAG_UT
88 UNTREATED
UNTREATED T knrm, VAG_UT
T%nrm, YAG_UT 88
88
87
87 I 87
0.90 1.0
1.0 1.1
1.1 1.2
1.2 1.3
1 .3 1.4 1.5
1.5 1.6 17
1.7
wavelength, pm
Wavelength, μm
Figure 8: Measured single surface transmission of NIR light through ARMs treated and thin-film coated YAG windows.

Established RIE/ICP etch processes were used to define both HYBRID-type and Motheye-type ARMs textures in one
surface of one-inch round, 6mm thick optical grade sapphire windows (99.99% purity) purchased from Crystal Systems,
Inc. of Salem Massachusetts. The windows were polished on both sides to a 60-40 scratch-dig specification with a
flatness of better than two waves measured in the red at 633nm. Figure 9 shows SEM images of the two types of ARMs
textures produced in sapphire windows used for process witness samples. On the left are elevation and overhead views
of the HYBRID ARMs texture where the tapered flat-top mesa structures are about 550nm high. Cone structures in the
Motheye texture shown on the right side in the figure are about 750nm high and extend over the full period at the base
for a high fill factor. The variable cone height is a result of over-etching this witness sample and was not observed in
the parts submitted for laser damage testing.
000a
.000a
0000I
I0000i
1P0000
0000a
i)OooG
O0OO

wwa e
raw

70°
0°
70°
0°

Figure 9: Elevation (70°) and overhead (0°) SEMs of NIR ARMs textures etched in the surface of two sapphire windows.

Figure 10 is a plot showing the measured transmission of the sapphire samples submitted to the pulsed laser damage
testing where as with the YAG data in Figure 8, the data has been normalized by referencing the single surface
transmission established by the widely published sapphire optical material constants. Two untreated sapphire windows,
S42UT and S44UT, show a flat transmission between 92.5 and 93% over the NIR spectrometer measurement range.
Motheye samples S30ME and S22ME represented by the black dashed and dotted curves in the figure exhibit broad-
band transmission averaging better than 99.5% over the 0.92-1.7
m range shown, with a transmission maximum at the
target 1064nm wavelength. A third Motheye window S32ME (thin solid black curve) has reduced performance but was
processed with a high degree of uniformity and a low defect count that is expected to be important for laser damage
resistance. Lastly, two sapphire windows were coated with the same single layer AR treatment applied to the YAG
windows by QTF, Inc. Because the refractive index of sapphire is lower than that of YAG, the thin film coated window
samples S41TF and S46TF, show peak transmission at a slightly shorter wavelength near 1
m, but still retain nearly
lossless transmission at the target 1064nm wavelength.

Proc. of SPIE Vol. 8016 80160T-6

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 loo
(Normalized)

100 100
1 00
S30ME --ARMs
S3OME ARMs

I 99 S22ME --ARMs
S22ME ARMs 99

98
98 98
El
Measured Transmission, %

S32ME --ARMs
S32ME ARMs
i
.
E
S 97

96-
96
m I
N T/ ,S41S48_TF
T%nrm, S41S46_TF
- 96
96
97

Diffraction
= 95-
U,
95
L
Loss T%nrm,
T%nrm, S22_ME
- - T%nrm,
S22_ME
S30_ME
T%nrm, S30_ME
S41S46TF --ARC
S41S46TF ARC - 95
95

0 94!j
94
Tt
Tt
nrm, S32_ME
T%nrm, S32_ME
nrm, Sapph_UT
T%nrm, Sapph_UT - 94
94

93
SAPPHIRE
SAPPHIRE 93
93
UNTREATED
UNTREATED
92 1064nm
1064nm - - 92
92

0.90
0.90 1.0
0 1.1 1.2
2 1.3
1.3 1.4
1 4 1.5
1 .5 1.6
1.6 17
1.7
Wavelength, pm
μm

Figure 10: Measured single surface transmission of NIR light through ARMs treated and thin-film coated sapphire windows.

ALON windows provided by Surmet Corporation were also textured with ARMs, characterized for transmission and
reflection, and submitted to laser damage testing. Transmission data for two Motheye textured windows, A29ME and
A30ME, are given as the black dotted and dashed curves in Figure 11. Again a thin-film AR coating was applied by
QTF to an ALON window A01TF, that exhibits high transmission at the target 1064nm wavelength as shown by the
solid grey curve in the figure.

l 00-
100 - I100
00
(Normalized)

C)

99-
99 A29ME
A29ME --ARMs
ARMs - 99
99

= 98-
98 - 98
98

I-
A3OME-ARMs
A30ME - ARMs
97- I 064nm . -- _JIb_alI4e.:;,:_?_: % -' I. '- 97
Measured Transmission, %

97 1064nm -
a 97

1 96-
96
- I:
- 96
96

IiE gs-
95 I: T%nrm,,A0I_TF
T% A01_TF AOITF --ARC
A01TF ARC
95
95
Diffraction
T%nrm,
T%nrm, A29_ME
A29_ME
0
94-
94 Loss
T%nrm,
T%nrm, A30_ME
A30_ME 94
94

--o 93-
93
tj
T%nrm, ALO
ALON_UT
N_UT
93
93

P 92
92 ALaN
ALON 92
92

C)
91-
91 UNTREATED
UNTREATED 91
91

900
9 90
90
0.90
0.90 1.0
1.0 1.1 1.2
1.2 1.3
1.3 1.4 1.5
1 .5 1.6
1.6 17
1.7
Wavelength.
Wavelength, pm
μm

Figure 11: Measured single surface transmission of NIR light through ARMs treated and thin-film coated ALON windows.

Lastly, single crystal quartz windows were processed with ARMs textures and characterized as shown in Figure 12.
100 100
(Normalized)

Q57ME - ARMs
99 99
Measured Transmission, %

98 98
T%nrm, Q57_ME
T%nrm, Quartz_UT

97 97
QUARTZ
UNTREATED
1064nm
96 96
0.90 1.0 1.1 1.2 1.3 1.4 1.5 1.6 1.7
Wavelength, μm

Figure 12: Measured single surface transmission of NIR light through untreated and ARMs treated Quartz windows.

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 4. PULSED LASER DAMAGE THRESHOLD MEASUREMENTS
At the 1064nm wavelength produced by solid state lasers based on neodymium-doped YAG, the pulsed LiDT of ARMs
textures in borosilicate glass and fused silica has been shown to be as high as 57 J/cm2 and 43 J/cm2 respectively, values
two to five times greater than the highest damage threshold values for thin-film AR coatings often reported in the
literature[24,25]. To test the damage threshold of the ARMs textured YAG, sapphire, ALON, and quartz samples, the
standardized pulsed LiDT testing service is provided by Quantel USA (formerly Big Sky Laser, Bozeman Montana)[26].
The tests conform to International Standards Organization (ISO) 11254, and involve exposing a statistically relevant
number of discrete locations (sites) over a sample surface to a calibrated level of laser energy with a specified
wavelength, pulse duration, and repetition rate. Referred to as an “S-on-1” test, the typical measurement exposes up to
100 sites to ten energy levels, 1 energy level per site to obtain a damage frequency verses energy level relationship. The
criteria for damage is a permanent surface change observed by visual inspection through a microscope configured for
150X magnification. A linear fit to the damage frequency verses pulse energy data establishes the LiDT.
Pulsed LiDT measurements of untreated (UT), ARMs-treated (ME), and thin-film AR coated (TF) windows were made
using a 10 nanosecond pulse width, 1064nm wavelength laser system at Quantel. Calibrated for a 420
m spot size,
Quantel exposed up to 100 sites on each sample where each site received 200 pulses, or shots, delivered at a rate of 20
pulses each second. Between 9 and 12 fluence levels were distributed amongst the 85-100 exposure sites over the
sample surface. Beginning with the ceramic YAG samples, two Yb-doped untreated samples (Y14UT and Y15UT)
were tested along with one untreated YAG window with no doping (Y29UT). Other than standard cleaning with
solvents and oxygen plasma, no special surface preparation method was used on the untreated YAG windows. Also
tested were two ARMs-treated Yb-doped YAG windows (Y11ME and Y13ME) and one ARMs-treated window with no
doping (Y26ME), and two Yb-doped YAG windows with thin-film AR coatings (Y16TF and Y17TF). The results from
each type of sample (UT, ME, TF) were averaged, and a linear fit to the data was made to obtain the curves shown in
Figure 13. A damage threshold of 11.0 J/cm2 was measured for the ARMs treated YAG samples (solid black
line/triangles), and a lower value of 7.3 J/cm2 was measured for the untreated YAG windows (solid grey line/open
crosses) – no significant difference was found between the doped and un-doped samples of each type. The low
threshold for damage found with the untreated YAG windows may be due to the simple commercial polish used to
prepare the windows. A more thorough polish may be needed to minimize sub-surface mechanical damage followed by
what is becoming standard practice in the high power laser component industry – a chemical etch to enhance the laser
damage resistance[27]. Residual sub-surface damage may have been partially removed by the plasma and wet chemical
etch processes used to form the ARMs textures in the YAG windows, possibly explaining why the ARMs textured
sample damage threshold was 50% higher than the untreated samples. Sub-surface damage may also have been
shielded by the additional material layer deposited on the thin-film AR coated samples, leading to the high damage
threshold of 21 J/cm2 observed for both Y16TF and Y17TF (open grey squares/dashed line).
2
Intensity, MW/cm 481 802 1123 1444 1764 2085 2405 2726 3047
100 100

Ceramic YAG
Damage Frequency, %

MOTHEYE = 11.0 J/cm THIN FILM ARC = 21.0 J/cm

2 2
80 80
Yb:YAG-Y11ME,Y13ME. YAG-Y26ME Yb:YAG-Y16TF,Y17TF

60 60

UNTREATED=7.3 J/cm
2

40 Yb:YAG-Y14UT,Y15UT. YAG-Y29UT 40

20 LiDT@1064nm, 10ns 20
20Hz, 0.42mm, Linear, TEM00
APRIL SPO, 85-95 sites, 200 shots/site
2011 Quantel USA Certificate #s 15599,1-8
0 0
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40
2
Fluence, J/cm
Figure 13: Results of a 1064nm LiDT test of untreated, ARMs-treated, and thin-film coated ceramic YAG windows.
The sapphire samples tested began with a much higher level of polish as provided by Crystal Systems, possibly leading
to the significantly higher damage thresholds measured. Two untreated sapphire windows (S42UT and S44UT), three
ARMs textured windows (S22ME, S30ME, and S32ME), and two thin-film AR coated windows (S41TF and S46TF)
were submitted for 1064nm damage testing at Quantel. Figure 14 shows the results where the thresholds for the ARMs
textured (solid black line/triangles) and untreated (solid grey line/open crosses) windows are comparable at 24.9 J/cm2

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 and 27.5 J/cm2 respectively. The thin film AR coated samples fared worse with a damage threshold of 16.7 J/cm2 -
about two-thirds the level of the Motheye samples.
Intensity, MW/cm
100 Intensity, MW/cm2
100 I!I!I!I!I! I 2
802
802 1123
1123 1444
I! I
1764
1764 2085
2085 2405
2405 2726
2726 3047
3047 3368 3688
3688 4009
4009
I100
00

SAPPHIRE
Damage Frequency, %

MOTHEVE = 24.9 27.5J/cm2

2 2
80-
80 MOTHEYE 24.9 J/cm2
J/cm UNTREATED
UNTREATED ==27.5 J/cm 80
80
U S22ME,S30ME,S32ME
822M F ,S3OM F ,S32M F S42UT,S44UT
542 UT, 544 UT
0)
60 60
80
0)

III
U-
O 40-
0)
40 THIN FILM ARC == 16.7
10.1 J/cm2
J/cm
2
40
S41TF,S46TF
541 TF.846TF --
-Ills
C
E
20-
20 I
I
L_J; LiDT@1064nm, iOns
LiDT@1064nm, 10ns 20
20
- 20Hz,
20Hz, 0.42mm,
SPO,
0,42mm.Linear,
85-110sites,
SF0.85-nc
Linear,TEM
sites,200
TEtts
00
200 shots/sits
shots/site -
APRIL 2011
APRIL 2011
Quantel USA Certificate
Certificate #s15599,15-21
#s 15599,15-21
0 0
0 2
2 4 66 8
8 10 12
1 14
14 it16 18
1 20
0 22 24 26 28 30
2
32 34 36 38 40
I
42
42 44
44
I

46
I I
48 50
50
I 0

Fluence, J/cm
Fluence, J/cm2
Figure 14: Results of a 1064nm LiDT test of untreated, ARMs-treated, and thin-film coated sapphire windows.

Four ALON windows and two Quartz windows were also damage tested at Quantel. The damage thresholds measured
for ALON are low compared to the sapphire, a result that may also be related to un-mitigated sub-surface polishing
damage. The single crystal quartz windows fared well with Motheye and untreated damage levels of 22.4 J/cm2 and
22.8 J/cm2 respectively. A chart summarizing all the damage testing results grouped by material, is given in Figure 15.

30
1064
1064nm
nm
PULSED LASER
LASER DAMAGE
DAMAGE THRESHOLD
THRESHOLD MEASUREMENTS
MEASUREMENTS

10ns,
iOns, 20Hz

20Hz 27.5
UT- UNTREATED

UNTREATED MOTHEYE

ME- MOTHEYE TF- THIN
TF- THIN FILM
FILM

UT
24.9

25
-
ME
ME
22.8
22.4

22.4
20.8
UT

Fluence, J/cm2

20
ME

TF

16.7
16.7

15
TF

TF
11.0

10
ME
ME

7.4
7.0

UT
5.7
ME
ME

5.9

5
UT
TFI
TF

CERAMIC
CERAMIC YAG
SAPPHIRE

SAPPHIRE CERAMIC ALON
QUARTZ
QUARTZ

Figure 15: Bar chart comparing the 1064nm LIDT results for the four materials tested.

5. SUMMARY
As an alternative to thin-film AR coating technology, AR microstructures continue to exhibit laser damage resistance
that can be equivalent to the durability of untreated material, levels 2 to 5 times higher than single or multi-layer AR
coatings. Studies focused on ARMs textures built in Raytheon ceramic YAG, show that surface polishing methods and
chemical etching prior to ARMs processing is critical for attaining the highest laser damage resistance. ARMs textures
in highly polished sapphire and quartz materials were produced with high transmission over a broad bandwidth in the
NIR combined with high levels of pulsed laser damage resistance measured using 10ns pulses at 1064nm. With further
work, ARMs technology can significantly enhance the power handling capacity and reliability of solid state lasers.

5. ACKNOWLEDGEMENTS
The authors thank Jeff Runkel of Quantel USA (JRunkel@quantelusa.com) for his fast and thorough work providing the
certified, NIST traceable LIDT testing results on more than 20 samples in less than 2 days. The SEM analysis was
performed by Mr. John Knowles at MicroVision Laboratories, Inc., (978-250-9909).

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