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Wavelength and temperature

dependence of continuous-wave laser


absorptance in Kapton® thin films

William J. Palm
Michael A. Marciniak
Glen P. Perram
Kevin C. Gross
William F. Bailey
Craig T. Walters

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Optical Engineering 51(12), 121802 (December 2012)

Wavelength and temperature dependence


of continuous-wave laser absorptance
in Kapton® thin films
William J. Palm Abstract. Optical properties and laser damage characteristics of thin-film
Air Force Research Laboratory aluminized Kapton® were investigated. Spectral absorptance of virgin and
Kirtland AFB, New Mexico 87117 irradiated samples was measured from the Kapton side of multilayered
insulation over 0.2 to 15 μm wavelengths at both room temperature
Michael A. Marciniak and 150°C. The laser-damage parameters of penetration time and max-
Glen P. Perram imum temperature were then measured in a vacuum environment at laser
Kevin C. Gross wavelengths of 1.07 and 10.6 μm. Differences in damage behavior at
William F. Bailey these two wavelengths were observed due to differences in starting
Air Force Institute of Technology absorption properties at these wavelengths. During laser irradiation, the
Department of Engineering Physics Kapton thin film was observed with a calibrated FLIR® thermal imager
Wright-Patterson AFB, Ohio 45433-7765 in the 8 to 9.2 μm band to determine its temperature evolution. Spectral
E-mail: michael.marciniak@afit.edu radiance throughout the mid- and long-wave infrared was also observed
with a Fourier transform spectrometer, allowing temperature-dependent
spectral emittance to be determined. Kapton emittance increased after
Craig T. Walters the material heated past approximately 500°C, and continued to increase
Craig Walters Associates as it cooled posttest. This evolving temperature-dependent spectral
Powell, Ohio 43065 emittance successfully predicts the increasing absorptance that led to
shortened penetration times and increased heating rates for the 1.07 μm
laser. For tests with constant absorptance and no material breakdown, a
simplified one-dimensional thermal conduction and radiation model
successfully predicts the temporally evolving temperature. © 2012 Society
of Photo-Optical Instrumentation Engineers (SPIE). [DOI: 10.1117/1.OE.51.12.121802]

Subject terms: laser heating; Kapton®; polyimide; spectral emittance.


Paper 120400SSP received Mar. 15, 2012; revised manuscript received Apr. 25,
2012; accepted for publication Apr. 25, 2012; published online Jul. 10, 2012.

1 Introduction wavelengths in other materials if the transient changes in


Prediction of laser-target thermal interaction is complicated absorptance in those materials are properly characterized.
by the transient nature of the target material’s properties as it Remote-sensing instruments like the Fourier-transform
undergoes laser irradiation. This research characterized the spectrometer (FTS) serve as valuable tools in determining
wavelength-dependent correlation between laser damage how laser coupling evolves and affects the prime damage
and initial laser absorptance by considering the primary mechanisms.
mechanisms for damage. Remote-sensing equipment was
2 Experiment
used before, during, and after laser irradiance testing to
analyze the transient temperature and absorption properties Thin-film samples of aluminized Kapton measuring
of thin-film aluminized Kapton® in a vacuum environment. 7.62 cm2 were irradiated at wavelengths in the near infrared
In this fashion, spectral data could be used to confirm evol- (NIR, 1.07 μm) (see Fig. 1) and long-wave IR (LWIR,
ving temperature results from calibrated FLIR® thermal 10.6 μm) (see Fig. 2). The film used for this experiment
images and compare them to evolving absorption trends dur- was constructed of a 50 μm-thick Kapton polyimide
ing material decomposition. As expected, laser absorptance with a thin aluminized back surface less than or equal
was determined to be the greatest contributing factor to mate- to 300 Å.
rial heating, but it was also observed to vary greatly with The tests were fully diagnosed with a full listing of
laser wavelength and irradiance and depend on the extent relevant diagnostic equipment.2 A small fraction of the
of Kapton decomposition.1 Absorptance measurements main beam was split off to form a diagnostic beam train
were made for the aluminized Kapton film before, during, for each laser. This diagnostic beam train is a known constant
and after irradiation at several laser irradiance levels. This fraction of the beam power and is collected in an integrating
work reports an independent spectral characteristic for each sphere with a thermopile detector that is linear over six
phase in the life of the irradiated material, yielding tempera- orders of magnitude with a 10-ms response time (shown
ture- and wavelength-dependent absorptance. Along with a in Figs. 1 and 2). The thermopile detector was calibrated
simple thermal model, this data may be useful for scaling daily to the power at the target plane using a Molectron
bulk material thermal interactions between various laser power meter. This technique ensured that the effects of
the optics and beam dumps were factored over a range of
powers. Irradiance was reported during the dwell time
0091-3286/2012/$25.00 © 2012 SPIE on each sample using a constant area of 23.75 cm2 and

Optical Engineering 121802-1 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

Fig. 1 Fiber laser beam train with beam splitters at the beginning and end of the beam train to measure power and spatial beam profile.

the calibrated power. The uncertainty is presented as the 3 Results


standard deviation of power measurements collected at Before irradiance testing, spectral reflectance for virgin
100 Hz during the dwell time. Spatial beam profile for the aluminized Kapton samples was performed from the Kapton
LWIR beam was determined using polymethylmethacrylate, side using a Varian Cary 5000 spectraphotometer and a
a typical profiling material that linearly ablates. The NIR Bomem MB157S FTS. The spectrum of the polyimide
laser followed the same setup, with an additional beam split- film at room temperature (∼25°C) is presented as spectral
ter placed at the final optic to minimize errors and provide absorptance in Fig. 4 and is identical to that measured at
a true replica of the beam profile at the target plane. The 150°C. These results are similar to previously reported
replica beam was imaged with a back-illuminated CMOS Kapton spectra.5,6
CCD video camera (shown in Fig. 2) and recorded to ensure The laser irradiance test data from the FLIR thermal
profile repeatability.3 Figure 3 depicts instruments involved imager were reduced using a MATLAB® curve fit developed
in analyzing the material interaction with reference to the from calibration elements produced within the FLIR
target plane. Strict control was used to calibrate the spectral ThermaCAM® RCal™ program in the 8 to 9.2 μm region,
effects of the vacuum chamber windows for the exterior a relatively flat, high-absorptance/emittance region as shown
instruments by performing a full radiometric analysis of in Fig. 4. The normalized interferograms from the FTS were
the path from the sample to the detector.4 imported into a MATLAB code that converted them into

Optical Engineering 121802-2 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

Fig. 2 CO2 laser beam train with two beam dumps and diagnostic beam splitting.

uncalibrated spectra. A linear relationship to known black- 4 Discussion


body calibration curves was then developed to yield The Kapton film responded as anticipated based on the pret-
calibrated apparent spectra with real units of radiance. est absorptance measurements at the two laser wavelengths.
After taking into account the vacuum chamber window At 10.6 μm, Kapton is highly absorptive, as are most organic
attenuation, true source radiance for both the spectral mea- materials, and the heating rate was high. At 1.07 μm, Kapton
surement and the thermal image was achieved. Figure 5 is fairly transparent, and heating rates were much lower for
shows example spectra of aluminized Kapton irradiated at the same irradiances. Temperature was recorded as a function
9.6  1.4 W∕cm2 in the NIR. The midwave infrared of time for each sample tested, and before major damage or
(MWIR) radiance, collected by the FTS’s InSb detector, decomposition, showed good correlation to a simple one-
is shown as a dashed curve, and the LWIR radiance, dimensional (1-D) conduction and radiation model. This
collected by the FTS’s HgCdTe (MCT) detector, as a dotted model involved a balance between estimated absorption
curve. The Planckian envelope was generated using the using derived values, 1-D conduction into the material,
FLIR-imager-inferred temperature (∼500°C here). This and radiation from the Kapton side only.
demonstrates the continuity achieved between the FTS Figure 6 presents the calibrated FLIR data for a 10.6 μm
and FLIR thermal imager when viewing the same sample laser irradiance of 2.98 W∕cm2 on the Kapton side of the
spot. Note that at 500°C, the spectral features observed at aluminized Kapton film. Two curves correspond to two
room temperature and the relatively flat, high-emittance frame integration times that are acquired alternately during
region of the LWIR remain. FLIR measurements. “FLIR Data 0” presents the FLIR data

Optical Engineering 121802-3 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

Fig. 3 Plan view sketch inside the vacuum chamber showing beam entrance and various diagnostic equipment locations.

Fig. 4 Spectral absorbance for 2-mil aluminized Kapton® at room temperature measured from Kapton side.

for a 3-ms integration time, which is valid for low tempera- due to the material’s low thermal diffusivity. Whereas the
tures before the detector saturates; the validity range for this test environment complicated the experimental setup, the
curve is 40°C to 250°C. “FLIR Data 1” presents the FLIR theory was greatly simplified by removing convection and
data for a 1-ms integration time and is valid for temperatures only treating 1-D conduction within the material and radia-
of 350°C to 700°C. To get a continuous curve for temperature tion from it. Based on the thermal diffusivity of Kapton, the
as a function of time, it was assumed that the transition characteristic distance for heat diffusion during a 60-s run is
between 250°C and 350°C was smooth and continuous about 2 mm. This and the appearance of the samples after
and could be represented by a parabolic splice, testing confirmed that there was no significant radial heat
conduction. However, thermal radiation from the front sur-
T ¼ −84.667t2 þ 383.12t − 4.044; (1) face played a dominant role in the temperature history of the
Kapton film at long run times with little Kapton decomposi-
with T in °C and t in seconds. The resulting continuous curve tion. This is illustrated by the FLIR thermal imager data com-
for temperature was then compared to a simple laser heat- pared to the 1-D thermal model, with radiation loss shown in
ing model. Fig. 7(a) for 1.07 μm laser irradiance of 7.31 W∕cm2 . A
The irradiance tests were conducted in a vacuum test Kapton thermal emittance of 0.41 in the 1-D thermal
environment which negated convective heat transfer. In model provides an excellent fit to the FLIR test data.
this environment, the dominant heat transfer mechanism is The thermal conduction model is a simple 1-D explicit
radiation, with very little conduction into the sample stand finite difference numerical solver with appropriate boundary

Optical Engineering 121802-4 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

specification for Kapton (0.71),7 which is probably valid


for room temperature or colder. The initial material proper-
ties for Kapton used in this analysis are presented in Table 1.
A similar comparison is made in Fig. 7(b) for 10.6 μm
laser irradiance of 2.98 W∕cm2 . Here, the agreement
between the FLIR data and the 1-D model is not quite as
good. Although irradiance is lower than in Fig. 7(a), higher
absorptance at 10.6 μm drives the temperature higher. The
early heating rate was empirically determined to be approxi-
mately 257°C∕s [straight dashed line in Fig. 7(b)], and the
absorptance derived from the early heating rate of 0.67
agrees to within 27% of the low-temperature steady-state
value at 10.6 μm (0.916, Fig. 4). The difference between
the FLIR data and the 1-D model seen between 2 and 6 s
may be an indication of an endothermic chemical reaction
within the material that slows the heating. Kapton has a
reported decomposition temperature of 525°C, a feature
Fig. 5 Calibrated source spectra of aluminized Kapton® undergoing that was observed in several different test cases.5 The perma-
1.07-μm laser irradiation at 9.6  1.4 W∕cm2 . Blackbody envelopes of nent discoloration of Kapton may begin slightly below this
each detector created for comparison using a Planckian curve fit at a
FLIR®-inferred temperature of approximately 500°C.
temperature after prolonged exposure above around 400°C.
(Note that this is not pyrolysis, or char formation which
occurs above 650°C). The effective thermal emittance
conditions. The front surface (Kapton side) was assumed to increased to 0.48 in this example, a faster heating scenario,
absorb heat equal to the irradiance multiplied by the absorp- based on the radiation-balance, conduction, and absorption
tance that was determined from the room-temperature mea- model. This modeled emittance value for the Kapton layer at
surements. Thermal radiation at the front surface was simply 650°C is not significantly different than that at 430°C [0.41,
assumed to follow the Stefan–Boltzmann law with a constant Fig. 7(a)] and will mostly depend on the level of discolora-
emittance. This emittance was adjusted to achieve a reason- tion in the material. The nature of the discoloration is not
ably good agreement with the data at long exposure times addressed here.
(near radiative equilibrium). No heat loss was assumed to The increased effective thermal emittance at higher
occur from the aluminized back surface, which has low emit- temperatures used in the heating model is consistent with
tance. As can be seen by the straight dashed line in Fig. 7(a), an increase in spectral emittance at temperatures above room
the early heating rate was empirically determined to be temperature measured by the FTS. FTS measurements
72°C∕s. This fit works well when there is no damage to during laser irradiation captured the change in spectral emit-
the material. The absorptance value of 0.076 used was tance with temperature and extent of surface discoloration.
derived from a fit to the early heating rate, where radiation Throughout a test, nearly constant spectral absorptance
was not significant. This derived absorptance agrees to was observed (as in Fig. 4) until the point where the Kapton
within 16% of the room-temperature steady-state value for surface starts to change color and decompose. Then, the
1.07 μm found pretest (0.09, Fig. 4). The emittance fit FTS-measured emittance increased in the MWIR and
value of 0.41 was lower than the manufacturer’s remained nearly constant in the LWIR. Owing to equipment

Fig. 6 Typical calibrated FLIR® data for two integration times. Curve “FLIR Data 1” represents the 1-ms integration, whereas “FLIR Data 0” the 3-ms
integration. The splice function between the two curves is represented with the data fit equation.

Optical Engineering 121802-5 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

Fig. 7 Comparison of FLIR® temperature data in a 1-D thermal model with front surface radiation loss for 1.07-μm (a) and 10.6-μm (b) laser tests.
Kapton® absorptance derived at 1.07 μm was 0.076 and that at 10.6 μm was 0.67. Kapton thermal emittance required for the fit was calculated to be
0.41 at 1.07 μm and 0.48 at 10.6 μm.

Table 1 Initial properties of Kapton® film.5,8 limitations, spectra in the NIR were not captured, but a
significant rise in emittance can be discerned by comparing
the material/laser interaction in terms of increasing heating
Material property Value for Kapton rates. Figure 8 shows pretest, real-time, and posttest spectral
emittance in the MWIR. The real-time (FTS InSb-detector–
Mass density (ρ) 1.42 g∕cm3
based) emittance flattened out in the MWIR region and then
Heat capacity (C p ) 1.09 J∕g C greatly increased after the sample was allowed to cool.
Figure 9 shows the pre- and posttest room-temperature
Thermal conductivity (k ) 1.2 × 10−3 W∕cm C Kapton spectral emittances from the NIR through the
LWIR. (Real-time data over this broader wavelength range
Thermal diffusivity (κ) 7.75 × 10−4 cm2 ∕s was not available.) Although the data in Fig. 9 do not include
the remote-sensing emittance data, an increase in MWIR
Absorptance at 10.6 μm from reflectance 0.916 absorptance was observed before cooling in the cases where
material discoloration or decomposition began. By extrapo-
Absorptance at 1.07 μm from reflectance 0.09 lating heating rate data between the two laser wavelengths
tested and normalizing the effects of absorption in the regime
Absorptance at 10.6 μm from initial heating data 0.67
before radiation becomes significant, we can infer a rise in
Absorptance at 1.07 μm from initial heating data 0.076 emittance for the 1.07 μm laser wavelength region of about
400%; that is, a starting material absorptance of 0.09 would

Optical Engineering 121802-6 December 2012/Vol. 51(12)

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Fig. 10 Empirical 3.8-μm absorptance of aluminized Kapton® derived


from FTS spectra captured during laser irradiation. Absorptance
increases during the heating process between approximately 0.2
Fig. 8 Comparison of pretest (room-temperature virgin) spectral and 0.4, and then increases to 0.63 in the decomposed (blackened)
emittance, spectral emittance measured during experimental decom- sample after it is cooled back to room temperature.
position (FTS InSb detector), and posttest (room-temperature decom-
posed) spectral emittance for a decomposed Kapton® sample.
5 Conclusion
These results demonstrate the unique wavelength- and tem-
perature-dependent material response that can be captured
with remote sensing techniques such as those used here.
This more-accurate characterization of the sample’s spectral
absorptance response then allows the scaling of laser test
results between laser wavelengths by using simple modified
heating models that better capture the true laser damage.
By using only initial heating rates from a calibrated FLIR
thermal imager and a simple 1-D thermal conduction model,
a reasonable measure of material absorptance for aluminized
Kapton was achieved at two laser wavelengths, 1.07 and
10.6 μm. FTS measurements demonstrated that trends in a
material’s spectral emittance may be captured for nondes-
tructive laser/material interactions using remote sensing
techniques. Here, emittance was most accurately captured
in the MWIR, so absorptance trends for aluminized Kapton
were charted at 3.8 μm. These results were consistent during
nondestructive testing and could be duplicated at any wave-
length in the MWIR. After a laser test, when the samples
Fig. 9 Comparison of aluminized Kapton® spectral absorptance were allowed to cool back to room temperature, aluminized
before and after laser irradiation to the point of decomposition.
Kapton absorptance increased dramatically.
The goal now is to use this varying-absorptance data
along with the thermal model to produce more-accurate pre-
increase to ∼0.4 after the material reached ∼500°C and
dictions of real-world transient conditions. Based on the data
decomposed. After the Kapton is allowed to cool, the acquired here, it should be possible to estimate the thermal
“decomposed” absorptance at 1.07 μm has increased by response of the Kapton to laser irradiation at wavelengths
roughly 10 times its virgin value. anywhere between 1 and 13 μm with greater accuracy
An empirical trend for aluminized Kapton absorptance at than was possible prior to this investigation.
increased temperatures due to laser irradiation can be estab-
lished using the real-time FTS data in the range of 3 to 4 μm,
where instrument gain is high and significant emittance Acknowledgments
changes were observed. Figure 10 plots 3.8 μm absorptance This work was supported by the High Energy Laser Joint
as a function of temperature and shows a slightly increasing Technology Office (HEL JTO) under grant AFOSR-BAA-
absorptance during testing, with a marked increase as the 2010-2 and was performed at Wright-Patterson AFB, OH.
decomposed material cools back to room temperature after-
ward. The absorptance variability during testing stems from References
the uncertainties in calibration and temperature extraction.
1. D. L. Decker, “Temperature and wavelength dependence of the reflec-
Although decomposition did occur near 500°C, the material tance of multilayer dielectric mirrors for infrared laser applications,”
experienced a significant absorptance rise at 3.8 μm after Laser Induced Damage in Optical Materials Proceedings Sponsored
cooling. A fully decomposed (blackened) sample at room by the National Bureau of Standards, NBS-SP-435, 230–235 (1975).
2. W. J. Palm et al., “Laser induced damage of Kapton thin films demon-
temperature had an absorptance of 0.63 at 3.8 μm. strating temperature and wavelength dependent absorptance: a case

Optical Engineering 121802-7 December 2012/Vol. 51(12)

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Palm et al.: Wavelength and temperature dependence of continuous-wave laser : : :

study in remote sensing material analysis,” Proc. SPIE 8190, 819009 Kevin C. Gross graduated from the Air Force
(2011). Institute of Technology (AFIT) with a PhD
3. C. T. Walters et al., High Energy Laser (HEL) Lethality Data Collection degree in physics in 2007. He joined the
Standards, Directed Energy Professional Society, Albuquerque, NM
(2007). AFIT faculty in 2008 and is currently is an
4. W. J. Palm, “Multilayer insulation laser damage characterization for assistant professor. He runs the AFIT
wavelength scaling,” MS thesis, Air Force Institute of Technology Remote Sensing Group and has been
(2011). involved in the collection of high-speed
5. W. N. Pollard and B. Hannas, “Non-contact temperature measurement radiometric, imagery, and spectroscopic
of aluminized polymer for space applications,” James Madison measurement of battle space combustion
University, Infrared Development and Thermal Testing Lab, VA signatures including high-explosive detona-
(2002). tions, muzzle flashes, rocket engines, and
6. M. J. Rowley, “Fiber-optic infrared measurement system for thermal
measurement of a Kapton® HN sample,” James Madison University, jet engine exhaust plumes.
Infrared Development and Thermal Testing Lab, VA (2003).
7. Dupont Kapton®, Polyimide Film General Specifications, www2
.dupont.com/Kapton/en_US/assets/downloads/pdf/Gen_Specs.pdf. William F. Bailey received a BS degree from
8. Product Data Specifications Sheet: Item No. MO09176, DE330, the United States Military Academy in 1964.
DE332, Dunmore Corporation (2007). He received an MS degree in nuclear physics
from the Ohio State University in 1966 and a
PhD from the Air Force Institute of Technol-
William J. Palm currently leads research and ogy (AFIT) in 1978. As a member of the AFIT
development of high-brightness fiber-based faculty since 1978, his research interests
laser systems and components for military include high-power lasers and microwave
applications on behalf of the Air Force systems, plasma dynamics and diagnostics,
Research Laboratory’s Directed Energy and characterization of hypersonic aerody-
directorate. He earned a BS in mechanical namic flows.
engineering from the University of Illinois
and a MS in applied physics from the Air
Craig T. Walters holds a PhD in physics from the Ohio State Univer-
Force Institute of Technology. He has
sity and has performed extensive research in the area of laser effects
published scientific work related to both
on materials. He currently has his own consulting firm, Craig Walters
lasers and spacecraft testing through
Associates, a small business devoted to providing R&D services and
the Directed Energy Professional Society, SPIE, AIAA, and the
consultation to industry and government in the areas of laser technol-
Aerospace Corporation.
ogy and electro-optics. He has performed contract research for other
small businesses as well as multibillion-dollar corporations in laser
Michael A. Marciniak received a BS degree application areas as diverse as laser cleaning and coating removal,
in mathematics-physics from St. Joseph’s laser beam diagnostics, optical system design, laser shock proces-
College, IN, in 1981, a BSEE degree from sing, laser-based inspection of adhesive bonds, laser-welding moni-
the University of Missouri-Columbia in 1983, tors, and high-power optical beam delivery systems. Prior to forming
and an MSEE (electro-optics) and PhD his own company, he had a distinguished thirty-year career at Battelle
(semiconductor physics) degrees from the Columbus Laboratories, culminating in eight years of service as a
Air Force Institute of Technology (AFIT) in Research Leader.
1987 and 1995, respectively. He is an associ-
ate professor in the Department of Engineer-
ing Physics at AFIT, with research interests in
various aspects of light-matter interaction,
including polarimetric scatterometry and thermal radiation of nanos-
tructured materials, optical signatures, and high-energy-laser damage
assessment.

Glen P. Perram received his BS degree from


Cornell University in 1980 and his MS and
PhD degrees from the Air Force Institute of
Technology (AFIT) in 1981 and 1986, respec-
tively. As professor of physics at AFIT, his
research interests include high-power gas
lasers, remote sensing, and laser-material
interactions.

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