NASA/TM--1998-208813

Effects of Ambient High Temperature Exposure

on Alumina-Titania High Emittance Surfaces

for Solar Dynamic Systems

Kim K. de Groh

Lewis Research Center, Cleveland, Ohio

Daniela C. Smith

Cleveland State University, Cleveland, Ohio

Donald R. Wheeler

Lewis Research Center, Cleveland, Ohio

Brian J. MacLachlan

Ohio Aerospace Institute, Cleveland, Ohio

Prepared for the

Space Technology and Application International Forum

sponsored by the Institute for Space and Nuclear Power Studies

Albuquerque, New Mexico, January 31-February 4, 1999

National Aeronautics and

Space Administration

Lewis Research Center

November 1998

https://ntrs.nasa.gov/search.jsp?R=19990021336 2018-05-11T16:57:47+00:00Z
Acknowledgments

The authors would like to thank David Roig of Cleveland State University for conducting high temperature

atomic oxygen exposures and Terry McCue of Dynacs Engineering for conducting the EDS analyses.

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Effects of Ambient High Temperature Exposure on

Alumina-Titania High Emittance Surfaces

for Solar Dynamic Systems

Kim K. de Groh 1, Daniela C. Smith 2, Donald R. Wheeler I , Brian J. MacLachlan 3

INASA Lewis Research Centel: Cleveland, OH 44135

:Cleveland State Universit).', Cleveland. OH 44121

-+Ohio Aerospace Institute. Cleveland. OH 44142

Abstract. Solar dynamic (SD) space power systems require durable, high emittance surfaces on a number of critical

components, such as heat receiver interior surfaces and parasitic load radiator (PLR) elements. To enhance surface

characteristics, an alumina-titania coating has been applied to 500 heat receiver thermal energy containment canisters and

the PLR of NASA Lewis Research Center's (LeRC) 2 kW SD ground test demonstrator (GTD). The alumina-titania coating

was chosen because it had been found to maintain its high emittance under vacuum (< 10 -'_torr) at high temperatures ( 1457°F

(827°C)) for an extended period (=2+700 hours). However, preflight verification of SD systems components, such as the

PLR, require operation at ambient pressure and high temperatures. Therefore, the purpose of this research was to evaluate

the durability of the alumina-titania coating at high temperature in air. Fifteen of sixteen alumina-titania coated Incoloy

samples were exposed to high temperatures (600°F (316°C) to 1500°F (816°C)) for various durations

(2 to 32 hours). Samples were characterized prior to, and after, heat treatment ['or reflectance, solar absorptance, room

temperature emittance and emittance at 1200°F (649°C). Samples were also examined to detect physical defects and to

determine surface chemistry using optical microscopy, scanning electron microscopy, operated with an energy dispersive

spectroscopy (El)S) system, and x-ray photoelectron spectroscopy (XPS). Visual examination of the heat-treated samples

showed a whitening of samples exposed to temperatures of 10(X)°F (538°C) and above. Correspondingly. the optical

properties of these samples had degraded. A sample exposed to 1500°F (816°C) for 24 hours had whitened and the thermal

emittance at 1200°F (649°C) had decreased from the non-heat treated value of 0.94 to 0.62. The coating on this sample had

become embrittled, with spalling offthe substrate noticeable at several locations. Based on this research it is recommended

that preflight testing of SD components with alumina-titania coatings be restricted to temperatures no greater than 600°F

(316°C) in air to avoid optical degradation. Moreover, components with the alumina-titania coating are likely to experience

optical property degradation with direct atomic oxygen exposure in space.

INTRODUCTION

Solar dynamic space power systems require durable, high emittance surfaces on a number of critical components such

as on the heat receiver interior surfaces and on the PLR elements. An alumina-titania coating, which has been evaluated

for SD heat receiver canister applications, has been chosen for PLR (an electrical sink for excess power from the

turboalternator/compressor (Shaltens, 1995)) applications due to its demonstrated high emittance and high temperature

durability in vacuum (de Groh, 1994). Under high vacuum conditions (< 10 .6 Iorr) the alumina-titania coating was lound

to bc durable maintaining a nearly constant emittance at a temperature of 1520°F (827°C) for ---2,700 hours as shown in

Figure I (de Groh, 1994). This coating has been successfully applied to the 500 thermal energy storage containment

canisters inside the heat receiver, and the PLR radiator (Figure 2), of the 2 kW solar dynamic ground test demonstrator

(Figure 3) at NASA LeRC. The SD GTD has successfully operated for over 500 hours in a LeRC's large thermal/vacuum

space environment facility, demonstrating the feasibility of solar dynamic power generation for space applications

(Shaltens, 1996a).

NASA/TM-- 1998-208813 1
0.8

oo

0.6

et_

0.4

E

UJ

0.2

(_) ....... =._._ ~..........

---+--- 0.025 mm

0.051 mm

|

1000 2000

Vacuum Heat Treatment Time (Hours)

3000

FIGURE 1. Emittance versus vacuum heat treatment (at 827 °C and 10-6 torr) time for two thicknesses of

alumina-titania coating on Haynes 188 substrates.

FIGURE 2. Parasitic load radiator of NASA Lewis' SD GTD system.

NASA/TM-- 1998-208813 2
Althoughthealumina-titania highemittanceoatinghasfunctionedsuccessfully inthe SD GTD system. SD flight PLR

hardware verification will require additional ambient pressure operation. This is needed in order to verify that the

electrical system and alternator control software function properly. PLR operation temperatures have been estimated to

be around 1200°F (649°C) under full load, with a maximum design temperature of 1500°F (816°C). If operation of the

PER in air causes a decrease in emittance, the PLR will operate at a higher temperature than desired while on-orbit. This

could shorten the PLR life, and possibly damage the system's elements. Therefore, the joint United States/Russian SD

flight demonstration (SDFD) project (Wanhainen, 1995) decided to test the high temperature durability of the aluminatitania coating in air. If degradation of the high emittance surface occurs with high temperature air exposure, it is critical

to determine what limitations (time/temperature) should be placed on operating the PLR in air prior to flight. It is also

important to determine whether any damage could be reversed through procedures such as heat treatment in a reduction

environment.

FIGURE 3. SD GTD system in the large space thermal/vacuum system at NASA Lewis

Research Center.

MATERIALS AND EXPERIMENTAL PROCEDURES

AlliedSignal Aerospace. the contractor for the power conversion unit and heat receiver, prepared sixteen test coupons for

durability evaluation. From an Incoloy 8(X) substrate, samples were cut to 1.2" x ! .2" squares and detonation gun flamesprayed at Praxair with 0.001"-0.002" thick alumina-titania coatings. The alumina-titania composition consisted of 60

wt e_ ALO_ - 40 wt e_ TiO_. Fifteen samples were heat treated in air for various durations and temperatures. Twelve

samples were exposed to the array of conditions corresponding to 600°F (316°C), 1000°F (538°C) and 1250°F (677°C)

lk)r4, 8.24 and 32 hours. Three samples were exposed to 15(R)°F (816°C) for 2, 8 and 24 hours. One sample was left

untreated as a control. Photographs (I.2X) and optical micrographs (12X and 101 X) were taken. The samples were

characterized for their optical properties (reflectance, absorptance and emittance). In addition, scanning electron

micrographs, EDS spectra and XPS spectra were obtained for both the control sample and the sample exposed to the

highest temperature for the longest duration (PLRI5) to compare surface morphologies and chemistries.

NASA/TM-- 1998-208813 3
Optical Properties

Solar integrated total (Pt), diffuse (Pd), and specular reflectance (Ps) were obtained using a Perkin-Elmer _,-9

Spectrophotometer operated with a 150 mm integrating sphere. Reflectance was measured from 250 nm to 2500 nm

and the data were convoluted into the air mass zero solar spectrum to obtain solar integrated values. With opaque samples

like these, the solar absorptance (ors) can be calculated by subtracting the integrated solar total reflectance from one.

Values for emittance at room temperature (F_,77OF) were obtained using a Gier Dunkel DB- 100 infrared reflectometer which

provides an integrated reflectance value which is then subtracted by I to get E77oF. Integrated thermal emittance at 1200°F

(649°C) values were calculated using the spectral total reflectance obtained from the 3,-9. Emittance was calculated by

first extrapolating the last 250 data points of the total reflectance curve (2250 data points) to higher wavelengths to

encompass 95% of the blackbody spectrum at 1200°F (649°C). This temperature was chosen because it was estimated

to be the maximum operating temperature of the PLR on-orbit. Based on the shape of the curve for the last 250 data points

from the _,-9, their root mean square (RMS) average was chosen for extrapolation. Next, the spectral absorptance was

calculated by subtracting the spectral reflectance from 1. Using Kirchhoff's law (Ex = (xx) the spectral emittance was

obtained (Siegel, 1981 ). The spectral emittance curve was then convoluted into the blackbody curve for 1200°F (649°C)

to give integrated thermal emittance at 1200°F (et20oor). While the extrapolation introduces uncertainty in the absolute

values, the data still yields valuable information by showing the overall change in emittance that was introduced due to

the heat treatment.

Surface Characterization

Overall photographs were taken with a Polaroid Landcamera. Optical micrographs were taken on an Olympus SZH

Stereo-zoom microscope. Electron micrographs were taken on a JEOL 840 Scanning Electron Microscope (SEM).

Energy dispersive x-ray spectrums were obtained using a Hitachi S-4700 Field Emission Electron Microscope operated

at 20 kV with an EDAX DX Prime system. X-ray photoelectron spectroscopy spectra were obtained on a

VG Scientific ESCA Lab MklI using nonmonochromatized AI K-alpha x-rays. The analyzed spot was 1 mm in

diameter. The peak areas were convened to atomic-percent (AT %) using sensitivity factors supplied by the manufacturer.

For surface cleaning or depth profiling, the sample was sputter-etched with 2.5 keV Ar ions rastered over a

3.5 mm by 3.5 mm area.

RESULTS AND DISCUSSION

The control and heat-treated samples are shown in Figure 4. Visual inspection of the samples indicates little degradation

of the originally blue-black surfaces at 600°F (316°C). At higher temperatures, pronounced whitening of the surface

coating is noticeable. At 1500°F (816°C), the coupons are essentially white and on sample PLR 15, exposed for 24 hours

at 1500°E embrittlement and spalling of the coating is observable (see Figure 5).

Figure 6 shows the influence of heat treatment on the reflectance of the PLR samples. Figure 7 shows the influence of

heat treatment on the emittance at 1200°E The results indicate that treatment at 600°F (3 ! 6°C) and i 000°F (538°C) did

not induce a significant change in reflectance or emittance. Only after heat treatment for 8 hours at a temperature of

1250°F (677°C) did a significant change occur. Table I is a summary of the optical data obtained. This table shows that

the emittance at 1200°F of sample PLR 15 Cheated |br 24 hours at 1500°F) is approximately 32% lower than the emittance

for the control sample. It is interesting to note that heat treatment does not affect room temperature emittance much, yet

has a large effect on the high temperature emittance. This is reflected in the _,-9 spectra, where larger increases in

reflectance are seen in the visible and less in the infrared wavelengths.

Electron microscopy revealed a significant change in the surface morphology of the coating with heating at 1500°F

(816°C) for 24 hours, as can been seen in Figure 8. Between the two cases, the heat-treated sample appears to be flatter,

with micro-cracks visible in the coating. The unheated coating remained electrically neutral during SEM imaging, but

the heated sample became electrically charged, indicating a decrease in the electrical conductivity with heating.

NASA/TM-- 1998-208813 4
Solar Dynamic PLR Emissivity Coatings

Air Operation Tests

1500_F. 2 hr_

600_F. 4 hr_ r_00_F - 8 hr_ 80_F - 24 hr_ 60@'F - 32 h_

1500"F - 8 hr_

R_00_F - 4 hrs IO00"F- 8 hrs

12,50'F - 4 hrs 1250_F _ 8 hv_

t000¢F - 24 hr_ 1000_F - 32 hrs

N N 12501 _ - 24 hrs 1250 _ - 32 h_

1500'F- 24 hr_

FIGURE 4. Alumina-titania coaled lncoloy samples after heat treatment at various temperatures

and times in air.

FIGURE 5. Sample PLR 15 showing coating embriulement and spalling after heat treatment at

1500 °F (816 °C) for 24 hours.

NASAFFM-- 1998-208813 5
0.8

¢1

to

0.6

to

n"

0.4

0

I--

0.2

0 .,i

--o-- 600OF

---e--- 1000 °F

--•-- 1250 °F

1500 °F

........: .........................................t ...................-:

0 5 10 15 20 25 30 35

Time (hours)

FIGURE 6. Total reflectance versus time for alumina-titania coaled lncoloy samples exposed to heat

treatment at various temperatures.

O

o 0.6

T"

tO

e"

0.4

E

LU

0.2

0

A ................ •

--*--- 600 °F

---=-- 1000 °F

--Jr-- 1250 °F

1500 °F

0 5 10 15 20 25 30 35

Time (hours)

FIGURE 7. Emittance at 1200 °F (649 °C) versus time for alumina-titania coated Incoloy samples

exposed to heat treatment at various temperatures.

NASA/TM-- 1998-208813 6
TABLE I. Optical Properties of Heat Treated Samples

Sample

Control

Treatment

UNTREATED

Pt

0.051

O_,,i

0.949

E'/7 ;I,:

0.884

_1")_)"1:

0.94

PLRI 4 hrs at 600 °F 0.059 0.941 0.889 0.94

PLR2 8 hrs at 600 °F 0.054 0.946 0.88 0.95

PLR3 24 hrs at 600 °F 0.058 0.942 0.875 0.94

PLR4 32 hrs at 600 °F 0.059 0.941 0.883 0.95

PLR5 4 hrs at 1000 °F 0.075 0.925 0.877 0.94

PLR6 8 hrs at 1000 °F 0.088 0.912 0.874 0.94

PLR7 24 hrs at t000 °F 0.077 0.923 0.852 0.94

PLR8 32 hrs at 1000 °F 0.076 0.924 0.86 0.94

PLR9 4 hrs at 1250 °F 0.09 0.91 0.872 0.93

PLR10 8 hrs at 1250 °F ().I.'M 0.846 0.884 0.89

PLRI 1 24 hrs at 1250 °F 0.206 0.794 0.854 0.83

PLR 12 32 hrs at 1250 °F 0.215 0.785 0.863 0.81

PLRI3 2 hrs at 1500 °F 0.304 0.696 0.838 0.71

PLR 14 8 hrs at 1500 °F 0.458 0.542 0.83 0.65

PLR 15 24 hrs at 15(X) °F 0.476 0.524 0.84 0.62

FIGURE 8. Surfaces morphologies of as-received and heat treated alumina-titania coated Incoloy samples. (a) Control

sample (unheated). (b) Sample PLRI5 heated at 1500 °F (816 °C) for 24 hours.

Because the heated samples appeared flatter in the SEM, the control sample and PLRI5 were scanned for average

roughness with a Dektak diamond stylus profilometer. The control sample had an average roughness of 5.6 + 1.2 t.tm

(3 scans), whereas the heated sample had an average roughness of 4.3 + 0.9 lam (4 scans).

Initial XPS analyses indicated that the as-deposited coatings were very high in C (48.5 AT % at the surface), even at sputter

depths that would normally remove surface C (20. I AT % at 43 nm depth). Because the coating surface is very rough,

the samples were decided to be sputter etched from 4 different angles for depth profiling, in an attempt to remove surfaces

that otherwise might be shielded if ion beam etching occurred from a single direction. Surface surveys and depth profiling

surveys (after etching from 4 directions) of the as-received coating and a heat-treated sample are listed in Table 2

and 3, respectively.

NASA/TM-- 1998-208813 7
TABLE2. XPSdepthprofileresultsfortheas-deposited coating

Element

Peak

Center (eV)

Surface

AT %

As-Deposited Coatin[_

1 nm depth

AT%

43 nmdepth

AT%

147 nmdepth

AT%

C 285.85 53.730 60.634 27.470 12.116

O 530.91 35.762 25.670 45.565 54.161

AI 74.00 5.455 6.927 15.566 20.994

Ti 458.72 3. I I 1 3.435 7.758 9.882

Pb 138.58 0.575 0.492 0.505 0.285

Zn 1021.60 0.476 0.247 0.092 0.066

Fe 712.00 0.204 1.106 0.914 1.259

Zr 182.5 0.192 0.516 0.642 0.494

Ca 347.14 0.160 0.349 0.675 0.474

Cu 932.60 0.160 0.266 0.191 I).229

K 294.85 0.144 0.208 0.0 0.0

A_ 368.0(/ 0.033 0.083 0.0 0.039

W 247.56 0.0 0.065 (I.622 0.0

TABLE 3. XPS depth profile results for heat treated sample PLR-15

ELement

C

O

AI

Ti

Pb

Zn

Fe

Zr

Ca

Cu

K

A_

W

Peak

Center (eV)

284.85

Heat Treated Sample (PLR-15)

Surface 1 nm depth 43 nm depth

AT % .AT% AT %

14.988 7.540 1.260

56.863 60.347 62.889

15. !88 17.041 19.986

147 nm depth

AT%

0.688

530.91 62.324

74.00 21.828

458.72 6.328 7.855 11.247 11.427

138.58 _233 0.472 _324 0.098

1021.60 _027 0.135 _084 0.0

712.00 _720 0.611 0.394 0.790

182.5 0.724 0.659 0.843 0.768

347.14 _220 0.252 0.332 0.390

932.60 _110 0.014 0.004 0.0

292.65 _806 0.915 0.335 0.216

368.00 _666 0.674 0.271 0.139

247.56 3.127 3.487 2.031 1.331

Even alter ion beam etching from 4 directions, the as-deposited coating was found to be high in C (60.3 AT % at 1 nm

depth). After etching to a depth of 147 nm, there was still a substantial amount of C present in the coating (I 2.1 AT %).

It is possible that carbon was incorporated in the coating from the acetylene gas used during the deposition process. Small

amounts of other "trace" elements such as Pb, Zn, Fe, Zr, Ca, Cu, K and Ag were detected. These trace elements are also

likely due to the detonation gun spray process. The AI and Ti peak centers (74.00 and 458.72, respectively) are consistent

with metal oxides and not elemental metals (Moulder). At a depth of 147 nm there was 54 AT % O, 21.0 AT % AI and

9.9 AT % Ti. It should be noted that after sputter etching to a depth of 147 nm where the C was mostly removed, the surface

still appeared black.

Heating the coating in air at 1500°F for 24 hours resulted in a significant loss of C (from 53.7 to 15.0AT % at the surface)

and a gain in O (from 35.8 to 56.8 AT %). The original "trace" elements changed in AT % slightly with heat treating,

and a significant amount of W is present in the heat-treated sample (3.1 AT %). The binding-energy peak centers for AI

and Ti did not change. But, a change of the Ti peak shape (two distinct peaks, one at 455.6 eV) was observed for the heattreated spectra at 147 nm depth, as compared to the as-received coating. By curve fitting for TiO2 and TiO, the as-received

coating appears to have a TiOJTiO ratio of = 1, and the heat-treated sample has a TiO2/TiO ratio of = 1.6. It should be

noted that TiC also has a peak at =455.0 eV (Moulder). It has been proposed that a change in oxidation state is responsible

for the optical property changes. Color changes associated with changes in the stoichiometry of alumina have been

reported by Arghiropoulos. The loss of oxygen during the coating process is believed to cause the white oxides to turn

NASA/TM-- 1998-208813 8
black. At a depth of 147 nm the heat-treated sample has only 0.7 AT % C compared to 62.3 AT % O, 21.8 AT % AI and

11.4 AT % Ti. These quantities are closer the those expected for AI203 (60%) -TiO2 (40%) which are 61.9 AT % O, 28.6

AT %, AI and 9.5 AT % Ti.

Energy dispersive spectroscopy, which is a deeper penetrating analytical lechnique ( 1-5 _m) than XPS ( 10- 100 ,_), was

conducted on the XPS sputter etched control sample to check if C was present in the bulk of the coating. The

as-received coating had 10.2 AT % C, 54.5 AT %, O, 24.9 AT % AI and 10.4 AT % Ti. This is in gotxl agreement with

the XPS analysis of the as-deposited coating at a depth of 147 nm. A SiC fiber was analyzed at the same time to verify

accuracy of the system. Carbon, which is present in the as-received coating has been oxidized and is thus not present

in the bulk of the heat-treated sample, and therefore may also play a minor role in the optical properties of the coating.

The emittance data suggests that ambient high temperature exposure is not a problem unless the coating is heated to

temperatures above I(XX)°F (538°C). Although no significant optical property changes were observed until 8 hours of

exposure at 1250°F (677°C), visible whitening and small changes in the reflectance and hence absorptance were observed

for samples exposed to 1000°F (538°C). This implies that the coating would not be stable at this temperature fi_r long

durations. Also, at around 1(X)0°F (538°C) titania undergoes a phase change which might exacerbate oxidation and cause

spalling of the coating (Leissler, private communication). This research indicates that the high temperature optical

property degradation of the alumina-titania coating is not likely reversible. The loss of C (which may play a minor role

in optical properties) from the coating is a permanent loss. It was proposed that if the oxides do gain some oxygen during

heating, exposure to a reduction environment apparently could reverse the degradation caused by oxidation. Yet, Praxair.

the coating supplier, has attempted reversal of the coating degradation using a hydrogen reduction environment but was

unsuccessful (Naim, private communication). Even if it was successful, this would not reverse the embrittlement and

spalling which occurred at 1500°F (816°C) after 24 hours. Arghiropoulos found reversible stoichiometric transformations in alumina at 932°F (500°C), and irreversible transformations at 1832°F (1000°C).

Based on this research it is recommended that components coated with the alumina-titania coating be operated at

temperatures of 600°F (316°C) or below in air. It is possible that there are temperatures above 600°F and below 1000°F

tk)r which the coating would be stable. However, further tests are necessary to determine a more precise failing

temperature and temperatures in this range were not investigated in this test program. The SD ground test demonstrator

PLR which is coated with the alumina-titania coating, has been operated for over 365 hours in air (Shaltens, 1996b). Even

at the maximum load (2kW) the heat generated by the PLR appears to be moderate (personnel could put their hands near

it during operation (Shaltens, private communication), and there has been no observable degradation of the coating. This

indicates that PLR operation temperatures might be lower than estimated and thus would not pose a threat to the optical

properties of the coating if operated in air.

Finally, it should be noted that based on this research, atomic oxygen (which is more reactive than molecular oxygen)

degradation is likely to be a concern for operation on orbit because the PLR panels will be directly exposed to the low

Earth orbit cnvironmcnt, unlike the heat receiver interior. The atomic oxygen durability of the coating therefore needs

to bc assessed prior to use of this coating on surfaces exposed to atomic oxygen impingement. Preliminary data obtained

on alumina-titania coated Haynes 188 substrates provided evidence of a significant decrease in optical properties with

high temperature ( 1520°F (827°C)) atomic oxygen exposure, as shown in Figure 9. The total plasma asher exposure

( 160 hours) was equal to a Kapton effective fluence of 5.8 x 1020 atoms/cm-" (or a performance requirement of 0.2 years

of sweeping ram atomic oxygen exposure on the International Space Station). Testing has not been conducted to see if

lower temperature atomic oxygen exposure would also cause optical property degradation.

SUMMARY AND CONCLUSIONS

Solar dynamic power system components, such as the parasitic load radiator, which are covered with a high temperature,

vacuum durable, high emittancc alumina-titania coating need ambient pressure operation in order to verify proper system

electrical function and to check out alternator control software of actual flight hardware. Sixteen samples of aluminatitaniacoated Incoloy were prepared for durability evaluation at high temperature in air. Fifteen samples were heat treated

at various temperatures for different durations. Visual examination of the samples indicated a whitening of the originally

blue-black coating upon exposure to 1000°F and higher. Degradation of the optical properties of the samplcs exposed

NASA/TM--1998-208813 9
®

='d

o

.O

<

¢.9

et_

E

t,H

0.95

0.90

0.85

0.80

0.75

0.70

0.65

0.60

0.55

0.50

k

o- . ......

"-----......~_

---e--- Emittance at 827 °C

---*--- Solar Absorptance

0 50 100 150 200 250

Atomic Oxygen Exposure (Hours)

FIGURE 9. Optical property degradation of atomic oxygen exposed alumina-titania coated Haynes 188

samples at elevated temperature.

to 1000°F or higher was verified through reflectance, absorptance and emittance changes. A sample exposed to 1500°F

for 24 hours appeared white, the thermal emittance at 1200°F decreased from 0.94 to 0.62, and the coating became

embrittled with spalling from the substrate observable in several locations. Based on this research it is recommended

that components with the alumina-titania coating be operated at temperatures of 600°F (316°C) or below in air prior to

space flight. Finally, the atomic oxygen durability of the coating appears to be a significant concern and needs to be

addressed prior to use of this coating on components directly exposed to the space environment.

REFERENCES

Arghiropoulos, B., et al., "'Reactivity of Non-Stoichiometrie Black Alumina," Proceedings of the 4th International Symposium on

the Reactivity of Solids, Amsterdam, May 30-June 4, 1960, p. 524-539.

de Groh, K. K., Roig, D. M., Burke, C. A. and Shah. D. R., "Performance and Durability of High Emittance Heat Receiver

Surfaces lbr Solar Dynamic Power Systems. NASA TM-106549, 1994.

Leissler, G., (NYMA. Inc.) Private Communication.

Moulder, J. E, et. al., Handbook of X-Ray Photoelectron Spectroscopy, Perkin-Elmer Corp., USA.

Naim, M. (Praxair), Private Communication.

Shaltens, R. K. & Boyle, R. V., "'Initial Results from the Solar Dynamic (SD) Ground Test Demonstration (GTD) Project at

NASA Lewis," 30 th IECEC, Orlando Florida, July 31-August 4, 1995, IECEC-95-42t. also NASA TM-1070(O.

Shaltens, R. K. and Mason, L. S., "500 Hours of Operational Experience from a Solar Dynamic Power System:' 31 _

intersociety Energy Conversion Engineering Conference, Washington, D.C., August I 1-16, 1996a, 1ECEC-96568:

also NASA TM-107294.

Shaltens, R. K, and L. S. Mason, "'Early Results From Solar Dynamic Space Power System Testing," NASA TM-107252. 1996b.

Shaltens, R. K., (NASA Lewis Research Center) Private Communication.

Siegel, R. and Howell J. R., Thermal Radiation Heat Transfer. Hemisphere Publishing Corporation, Washington, 2nd ed.. 1981.

Wanhainen, J. S. and Tyburski, T. E., "Joint US/Russian Solar Dynamic Flight Demonstration Project Plan:" IECEC Paper No.

AP-176. ASME, 1995, pp. 417-420

NASA/TM-- 1998-208813 I0

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November 1998 Technical Memorandum

4. TITLE AND SUBTITLE 15. FUNDING NUMBERS

Effects of Ambient High Temperature Exposure on Alumina-Titania

High Emittance Surfaces for Solar Dynamic Systems

6. AUTHOR(S)

Kim K. de Groh, Daniela C. Smith, Donald R. Wheeler, and Brian J. MacLachlan

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES)

National Aeronautics and Space Administration

Lewis Research Center

Cleveland, Ohio 44135-3191

9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES)

National Aeronautics and Space Administration

Washington, DC 20546-0001

WU-632-1 A- ! E

8. PERFORMING ORGANIZATION

REPORT NUMBER

E-I1412

10. SPONSORING/MONITORING

AGENCY REPORT NUMBER

NASA TM--1998-208813

11. SUPPLEMENTARY NOTES

Prepared for the Space Technology and Application International Forum sponsored by the Institute for Space and Nuclear

Power Studies, Albuquerque, New Mexico, January 31-February 4, 1999. Kim K. de Groh and Donald R. Wheeler, NASA

Lewis Research Center; Daniela C. Smith, Cleveland State University, Cleveland, Ohio 44115; Brian J. MacLachlan, Ohio

Aerospace Institute, 22800 Cedar Point Road, Cleveland, Ohio 44142. Responsible person, Kim K. de Groh, organization

code 5480, (216) 433-2297.

12a. DISTRIBUTION/AVAILABILITY STATEMENT

Unclassified - Unlimited

Subject Categories: 20 and 27 Distribution: Nonstandard

This publication is available from the NASA Center for AeroSpace Information, (301) 621-0390.

12b. DISTRIBUTION CODE

13. ABSTRACT (Maximum 200 words)

Solar dynamic (SD) space power sysfems require durable, high eminanee surfaces on a number of critical components, such as heat receiver interior

surfaces and parasitic load radiator (PLR) elements. To enhance surface characteristics, an alumina-titania coating has been applied to 500 heat receiver

thennal energy containment canisters and the PLR of NASA Lewis Research Center's (LeRC) 2 kW SD ground test demonstrator (GTD), The aluminatitania coating was chosen because it had been found to maintain its high emittance under vacuum (_<10_ torr) at high temperatures ( 1457°F (827°C)) for

an extended period (=2,700 hours). However, preflight verification of SD systems components, such as the PLR. require operation at ambient pressure

and high temperatures. Theretore, the purpose of this research was to evaluate the durability of the alumina-titania coating at high temperature in air.

Fifteen of sixteen alumina-titania coated lncoloy samples were exposed to high temperatures (6(K)°F (316°C) to 1500°F (816°C)) for various durations

(2 to 32 hours). Samples were characterized prior to, and after, heat treatment for reflectance, solar absorptance, room temperature emittance and

emittance at 1200°F (649°C). Samples were also examined to detect physical defects and to determine surface chemistry using optical microscopy,

scanning electron microscopy, operated with an energy dispersive spectroscopy (EDS) system, and x-ray photoelectron spectroscopy (XPS). Visual

examination of the heal-treated samples showed a whitening of samples exposed to temperatures of 1000°F (538°C) and above. Correspondingly. the

optical properties of these samples had degraded. A sample exposed to 1500°F (816°C) for 24 hours had whitened and the thermal eminance at 1200°F

(649°C) had decreased from the non-beat treated value of 0.94 to 0.62. The coating on this sample had become embrittled, with spalling offthe substrate

noticeable at several locations. Based on this research it is recommended that preflight testing of SD components with alumina-titania coatings be

restricted to temperatures no grealer than 600°F (316°C) in air to avoid optical degradation. Moreover, components with the alumina-titania coating are

likely to experience optical property degradation with direct atomic oxygen exposure in space.

14. SUBJECT TERMS

Solar dynamic system; Thermal emittance; Solar absorptance; Alumina-titania; Heat treatment:

Ambient pressure: High temperature durability: Solar dynamic ground test demonstrator

17. SECURITY CLASSIFICATION

OF REPORT

Unclassified

NSN 7540-01-280-5500

18. SECURITY CLASSIFICATION

OF THIS PAGE

Unclassified

15. NUMBER OF PAGES

16

16. PRICE CODE

A03

19. SECURITY CLASSIFICATION 20. LIMITATION OF ABSTRACT

OF ABSTRACT

Unclassified

Standard Form 298 (Rev. 2-89)

Prescribed by ANSI Std. Z39-18

298-102