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PHYSICS

AUBURN UNIV1 RSI'

AUBURN, ALABAMA

NASA-CR-178712) SURFACE ANALiSIS OF SPACE

lEL2SCOt£ HAIIBItl SPECIMENS fital Report

Auburn Univ.) liO F HC ACb/KF Aul CStL 03A

N86-22U60
SURFACE ANALYSIS OF SPACE TELESCOPE

MATERIAL SPECIMENS

(H-78184B)

Final Report prepared for

GEORGE C. MARSHALL SPACE FLIGHT CENTER

Marshall Space Flight Center, AL 35812

June 15, 1985

by

Albert Thomas Fromhold

Department of Physics

Auburn University, AL 36849
SURFACE ANALYSIS OF SPACE TELESCOPE MATERIAL SPECIMENS

(H-78184B)

FINAL REPORT

(June 15, 1985)

Albert Thomas Fromhold, Jr.

Department of Physics

Auburn University, AL 36849

Prepared for

George C. Marshall Space Flight Center

Marshall Space Flight Center, Alabama 35812
FINAL REPORT

NASA Contract H-78184B

entitled

"Surface Analysis of Space Telescope Material Specimens"

Principal Investigator:

Co-Investigator:

Dr. Albert T. Fromhold, Jr.

Physics Department

Auburn University, AL 36849

Dr. Kasra Daneshvar /""^

Physics Department

Auburn University, AL 36849

ABSTRACT

Qualitative and quantitative data on Space Telescope

materials which were exposed to low earth orbital atomic

oxygen in a controlled experiment during the 41-G (STS-17)

mission were obtained utilizing the experimental techniques

of Rutherford backscattering (RBS), particle induced x-ray

emission (PIXE), and ellipsometry (ELL). The techniques

employed were chosen with a view towards appropriateness for

the sample in question, after consultation with NASA

scientific personnel who provided the material specimens. A

group of eight samples and their controls selected by NASA

scientists were measured before and after flight.

Information reported herein include specimen surface

characterization by ellipsometry techniques, a determination

of the thickness of the evaporated metal specimens by RBS,

and a determination of trace impurity species present on and

within the surface by PIXE. The work described was

undertaken for a firm-fixed price of $9900, which included

use of the experimental facilities of Auburn University. The

imputed costs to Auburn University greatly exceeded this

amount.
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INTRODUCTION

Experimental studies were made on eight flight metal

specimens and on the corresponding eight control metal

specimens both before the STS-17 (41-G) shuttle mission and

also after flight. These data are discussed in detail in

this report, which is divided into sections entitled Visual

Observations, Ellipsometry Data, Rutherford Backscattering

Measurements, and Proton-Induced X-Ray Emission. The

conclusions reached on the basis of each of these techniques

are listed in that section of the report. Recommendations

for fu'ture studies are listed at the end of the report.

The purpose of the measurements described in this report

was to ascertain the effects of exposure of the metal

specimens to the space ambient in low earth orbit. The

primary reactive species during exposure is the atomic oxygen

produced by ultraviolet decomposition of the low pressure

molecular oxygen which otherwise would be present at that

altitude.

The data obtained in this study are for various metal

specimens chosen by NASA scientists for this study. The

specimens were evaporated layers of silver, gold, palladium,

platinum, nickel, copper, aluminum, and chromium on metal

substrates. The nominal thicknesses of the layers ranged

from 500 to 5000 A. More quantitative values for the

thicknesses were deduced in this study.

VISUAL OBSERVATIONS AFTER FLIGHT

Silver:

The control sample had a milky white appearance. The

flight sample had a brownish color with more texture to it

than the control sample. There were sharp differences in the

appearance of the silver surface underneath the tabs holding

the flight sample, since the tabs protected the underlying

silver. Specifically, there were interference color rings

proceeding outward in a concentric elliptical pattern,

indicating a successively thicker surface layer as one

proceeds from the most protected part of the silver surface

towards the fully exposed part of that surface. There were

no such interference colors under the tabs of the control

sample.
Gold:

There were no visual differences between the control and

flight specimens.

Palladium:

Although the differences in appearance of the control

and flight specimens were slight, nevertheless the flight

sample appeared less bright, and had a more milky tint.

Platinum:

There were no visual differences between the flight and

control specimens.

Nickel:

There were no visual differences between the flight and

control specimens.

Copper:

The flight specimen had a brown-colored appearance

relative to the control specimen. Underneath the tabs

holding the flight specimen, however, where the copper

surface was protected from exposure, the surface had the same

appearance as the surface of the control specimen.

Aluminum: .

The flight sample may have a slightly more milky

appearance than the control specimen.

Chromium:

There were no visual differences between the flight and

control specimens.
- 4 -

ELLIPSOMETRY DATA

Introduction

A complete set of optical constant data were measured on

the eight flight metal specimens and on the corresponding

eight control metal specimens both before the STS-17 (41-G)

shuttle mission and also after flight. These data, which are

listed in Table 1, are discussed in detail in this section

The purpose of the measurements was to ascertain the effects

of exposure of the metal specimens to the space ambient in

low earth orbit. The primary reactive species during

exposure is the atomic oxygen produced by ultraviolet

decomposition of the low pressure molecular oxygen which

otherwise would be present at that altitude.

The data obtained in this study are presented in a

series of bar graphs depicting the value of the optical

refractive index n and the optical absorption coefficient k

for the various metal specimens chosen by NASA scientists for

this study. The specimens were evaporated layers of silver,

gold, palladium, platinum, nickel, copper, aluminum, and

chromium on metal substrates. The nominal thicknesses of the

layers ranged from 500 to 5000 A, with more quantitative

values for the thicknesses as deduced from our RBS data

listed in Table 2. The intense mercury green line (5461 A)

was employed for the measurements.

Experimental Results from Ellipsometry

In order to facilitate the interpretation of the data,

it is worthwhile to describe the several types of information

which are contained in the figures, and explain how this

information can be extracted readily from the three different

types of figure utilized. First of all, let us describe our

so-called "standard" plot, an example of which is given in

Fig. 1. A standard plot contains eight individual bars on a

graph. Each standard plot is for one optical constant on one

sample taken either prior to flight or following the flight.

The optical refractive index or the optical absorption

coefficient which is represented by each of the eight bars in

a standard plot will be described more specifically below.

Such a plot can depict either the refractive index n or the

absorption coefficient k for a given elemental metal, and all

data on the plot are either pre-flight or else post-flight.

Such standard plots as described above are presented in

pairs in a large number of figures in this report for the

purpose of drawing comparisons and obtaining other

information. In each plot, data are presented for two

samples of the same elemental metal. Data prior to flight

for the two samples are designated as A and B, respectively.
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One of the two samples was subsequenntly flown and exposed on

the STS-17 mission, this sample being the one represented as

B. The other of the two samples, namely the one represented

as A, is the control. Post-flight data on these two samples

are designated by F for the flight sample (B before flight)

and C for the control sample (A before flight). Thus we have

the correlation:

BEFORE FLIGHT AFTER FLIGHT

SAMPLE:. A =========>

SAMPLE: B =========>

A given standard plot contains either A,B data or else

C,F data, but is restricted to either n data or k data. On a

given figure containing two such standard plots, four types

of figure based on the various combinations would therefore

be possible. However, we have found it useful to restrict

the figures to the following three combinations.

BEFORE FLIGHT AFTER FLIGHT

n: A,B + C,F

k: A,B + C,F

The main purposes of the various figures will now be

explained. .Standard plot pairs illustrating n and k (n,k

pairs) for a given metal before flight (A,B) indicates the

overall quality of the samples, since at that point in time

the data for the two specimens of a given metal should not

differ in any essential way. Eight figures (Figs. 2 through

9) illustrate these results for the eight elemental metals

utilized in this study.

On the other hand, standard plot pairs illustrating

either n or else k for a given elemental metal before and

after the flight serve two important purposes. First of all,

comparison of the A and C data demonstrates the aging effect

on the optical constants during the several weeks time period

spanning the STS-17 mission. This aging effect must of

course be factored into any changes noted in the flight

sample during this period. Comparison of the B and F data in

juxtaposition with the A and C data then allows one to deduce
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the specific effects of exposure during the shuttle flight on

the metal specimen in question. There are AB,CF plot pairs

for each of the two optical constants of a given metal. With

8 different elemental metals, this gives rise to 16 figures

which will be discussed below in this report.

Other types of figures are also used in this report to

deduce important correlations and inclusions from the

ellipsometry data. Some of these figures are made up of

plots which are averages of the data presented in the

standard plots. Before these figures can be explained, it is

necessary to describe in greater detail the actual data

contained in a given standard plot. To do this, it is

helpful to refer to a specific standard plot. Fig. 1 gives

the refractive index data for the two samples of chromium

before the flight. The letters A and B denote the sample in

question. Two of the four bars for sample A give the results

of two independent determinations (labeled a and b) for a

given position on the sample surface^ and the other two bars

for sample A give the results of two independent

determinations (again labeled a and b) for a different

position on the sample surface. The two positions on the

sample surface are labeled 1 and 2, respectively. Good

agreement between the a,b data for a given position gives

confidence in the experimental precision of the measurement;

good agreement between the data for positions 1 and 2 gives

us confidence that the surface of the sample is homogeneous.

(The sample surface actually includes the region of

penetration of the light wave, which typically can be 500 A

into the bulk of the metal.) The need for precision requires

no explanation. The need for surface homogeneity is less

specific since it is based on several considerations, one

being general confidence in good sample preparation and

another being the pragmatic consideration that there is no

way to preserve an accurate memory of the area measured after

the sample is removed from the ellipsometer. That is, the

measurement does not mark the area physically, so once the

sample was removed from the ellipsometer and subsequently

returned for remeasurement, one must rely on the fact that

the values obtained are characteristic of any part of the

surface. In summary, agreement between the data labeled A.la

and A.lb demonstrates measurement precision, as also would

the agreement between the data labeled A.2a and A.2b.

Agreement between the A.I and A.2 data demonstrates sample

homogeneity. Exactly analogous statements can be made for

the B data shown in the same standard plot, since that data

is the corresponding data for the second of the two samples.

Agreement between the A and B data gives us the required

confidence that prior to the shuttle flight the control and

flight samples are essentially the same, and if not exactly

the same, at least we quantify the differences between the

two samples. This represents a basic requirement for drawing

meaningful conclusions by comparing the data on the two
samples after flight. It can be inferred from the standard

plot for the refractive index of chromium shown in Fig. 1,

for example, that the data are precise (compare A.la and

A.lb, compare A.2a and A.2b, compare B.la and B.lb, and

compare B.2a and B.2b), the surface is homogeneous (cf. A.I

and A.2 data, and also B.I and B.2 data), and the two samples

are essential identical in optical properties (compare A data

with B data). It is clear that these conclusions bear the

restriction that they are limited to the refractive index

data, so it is necessary to make a similar comparison of the

absorption coefficient data.

, Each, of the eight figures (Figs. 2 through 9) thus

gives us in an analogous way a more or less complete picture

of the optical quality of the sample it represents. It may

be noted from these figures that the experimental precision

is excellent for all eight specimens, and the surface

homogeneity varies from excellent for Cr, Pt, Pd, and Al to

very good for Cu, Pd, Au, and Ag. As might be expected,

there is somewhat more variation in the sample-to-sample data

for a given metal, though as already noted the data for the

chromium samples are in excellent agreement. The sample to

sample agreement for Au, Pd, and Ni is quite good, as can be

noted from Figs. 3, 4, and 6 that for copper and aluminum is

relatively good, as can be noted from Figs. 7 and 8. For Pt

the agreement is quite good for the refractive index but

there is a sample to sample difference of about 15% for the

absorption coefficient (see Fig. 5). For silver (see Fig.

2) the agreement for the absorption coefficient from sample

to sample is within about 5%, but there is a factor of 2

difference in the refractive index between the two samples.

Although this difference is somewhat surprising, such

differences are not uncommon in the literature. (For

example, values which have been cited for the refractive

index of silver vary from 0.066 to 0.240 to 3 at wavelength

6328 A.) More importantly, our observed difference turned out

to be of the same order as the aging effect, which in turn

was relatively small compared to the much larger changes

which occurred upon exposure to the shuttle environment in

orbit.

Figures 10 through 25 depict the effects of the shuttle

flight exposure on the samples. Each figure contains two

standard plots for the same optical constant of the same

elemental metal. The standard plot in the upper half of the

figure shows the pre-flight data, and the standard plot in

the lower half of the figure shows the post-flight data. A

study of these figures shows that by far the greatest changes

which can be attributed to exposure to space environment

occur for silver (see Figs. 10 and 11), these changes being

very large for both the refractive index and for the

absorption coefficient. Figures 14, 15, 20, 21, 24, and 25

show that changes in both optical constants because of space

exposure also occur for palladium, copper, and chromium,
- 8 -

although the effects are not as large as for silver, and

likewise but to a somewhat lesser extent in gold and

aluminum. There was also a change in the refractive index of

platinum (Fig. 16), but this was of the same order as the

sample to sample variation in the absorption coefficient of

platinum prior to flight (Fig. 17). Thus it can be said

that all eight metals show some effects which can be

attributed to flight exposure. These effects are analyzed

somewhat more quantitatively below.

Utilizing the fact that the precision of the

measurements taken on a given area of each sample at a given

time was extremely good, an averaging of these data was

carried out and plots were made in which the averaged data

for the two spatial sites on a given sample are given as

adjoining bars. Also included in this new series of plots

are both A,B and C,F data for either n or else k. This type

of plot differs of course from the standard plots described

above and utilized to this point. On a given figure we

include both the n data plot (upper half) and the k data plot

(lower half of the figure). These results for the 8

elemental metals are shown in Figs. 26 through 33. A

comparison of the A and C data in a given plot shows, for

example, the aging effects in the control specimen over the

weeks spanning the mission, whereas a corresponding

comparison of the B and F data includes aging but shows

especially the much larger effects produced by flight. It

can be noted from Fig. 26 that the aging effect on the

refractive index of silver was a factor of 2, as noted by

comparing the A and C data, whereas the corresponding change

due to exposure (including aging) of the flight sample was a

factor of 8. It can be noted from Fig. 33 that chromium

also underwent a significant aging effect. Nickel, copper,

-and aluminum also exhibited aging effects (see Figs. 30

through 32), whereas no aging effects could be noted for gold

(see Fig. 27 and only minor aging occurred in palladium and

platinum (Figs. 28 and 29).

A comparison of the A and B data in these plots (Figs.

26 through 33) also shows convincingly that the sample to

sample variations are significantly smaller than the

variations produced by exposure during flight as indicated by

a comparison of the C and F data. For example, Fig. 27 for

gold shows small sample to sample variations in n and k

compared to the changes in n and k which can be attributed to

flight exposure.

To emphasize the especially large space exposure effects

observed for silver relative to the other metals, a separate

figure (Fig. 34 shows the flight sample results for the

refractive index for both gold (upper half) and silver (lower

half of the figure). The 10% or so variation in n for gold

due to flight exposure seems rather small compared to the

factor of 8 or so variation in n for silver during the same

flight exposure.
- 9 -

The data presented in the adjoining bars in Figs. 26

through 33 discussed above clearly demonstrate that we do not

need to worry about nonhomogeneity in the surface of a given

sample. Thus the data for a given sample taken at a given

time can be averaged, and these averaged data can be used to

make a closer comparison between data taken on a given metal

specimen before and after flight. This gives us our finest

representation of the effects of flight exposure on each of

the elemental metals. In this third type of graph, the data

for n or for k for a given sample are presented as adjoining

bars, one bar denoting the pre-flight measurements and the

other denoting the post-flight measurements. On a given

plot, the data for both samples of a given elemental metal

are given so that one has a comparison of the pre-flight and

post-flight data on the flight specimen with the

corresponding data on the control specimen. The n plot is

then given as the upper half of the figure and the k plot is

given as the lower half of the figure. These eight figures

for the eight elemental metals are Figs. 35 through 42. By

examining carefully these figures, one can see that the

adjoining bars for the control specimen (denoted in this

third type of plot as C before flight and C" after flight) do

not differ very much from one another, thus showing that

aging effects are really quite unimportant with the possible

exception of n for silver. On the contrary, the adjoining

bars for the flight specimen (denoted as F before flight and

F

1 following flight) demonstrate the experimentally

significant changes which occurred in the flight specimen

during the STS-17 mission.

Although this completes our discussion of the

ellipsometer results, it is interesting to show composite

figures for the optical constants for the entire series of

elemental nj.etals in this study. Figures 43 through 46 show

these data for both n and k before the flight and after the

flight. One cannot help but note how much the optical

constants differ from metal to metal, differences which are

generally far greater that the variations from sample to

sample of the same elemental metal and the variations which

can be attributed to exposure to space environment. The

exception to this general observation is silver, which under

space exposure takes on optical characteristics which could

be typical of some entirely different metal.
- 10 -

RUTHERFORD BACKSCATTERING MEASUREMENTS

Introduction

The objectives of the RBS measurements were to determine

the sample thickness before flight as an independent check on

the thickness deduced from the evaporation monitor, and to

ascertain whether any significant surface layers were formed

during flight or whether any significant decreases in

thickness due to surface erosion occurred during flight.

Figure 47 illustrates the sample thicknesses obtained prior

to and following the flight. These thicknesses are also

listed in Table 2. A comparison of the RBS data taken after

flight with that taken before flight shows some differences,

but these differences are for the most part not systematic

enough or sufficiently large to be considered statistically

significant, with the possible exception of silver where a

40% increase in thickness was indicated for the flight

specimen.

The primary RBS data are given in Figs. 48 through 79.

These figures were used to obtain the thicknesses shown in

Fig. 47, and in addition, they illustrate a number of

interesting qualitative effects.

RBS Results for Silver:

The RBS spectrum for the Ag control and flight samples

before the flight are shown in Figs. 48 and 49. The width

of the tall peak on the right side of the figure is used to

deduce the thickness of the silver layer. (These are the

thicknesses which are listed in Table 2; note that they are

initially in the range of 2300 angstroms.) The portion of the

spectrum to the left in the figure is produced by the

substrate, which in the present case is aluminum,as confirmed

by the PIXE data. The spectra of the two samples can be

noted to be essentially the same at this point in time,

namely, prior to the shuttle flight. The corresponding

spectra measured after the flight are shown in Figs. 50 and

51. Notice first of all that the two spectra after the

flight are qualitatively quite different. Then note by

comparison of Figs. 50 and 51 after the flight with

corresponding data before the flight (Figs. 48 and 49) that

the control sample manifests the same qualitative spectra

before and after flight, whereas the flight sample manifests

quite different qualitative spectra before and after the

flight. The conclusion, of course, is that exposure of the

silver to the atomic oxygen atmosphere in low earth orbit

produces large changes in the silver. A comparison of the

spectra after flight (Figs. 50 and 51) shows three distinct

effects:
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(a) The flight spectrum indicates a silver layer which

is thicker physically than that of the control

specimen.

(b) The region of the flight spectrum produced by the

silver is rounded instead of being squared off,

which indicates nonhomogeneity of the silver near

the interfaces.

(c) The portion of the flight spectrum produced by the

substrate is more rounded than that of the control

specimen, which indicates the presence of oxygen in

the silver.

The thicknesses of the flight and control samples

obtained from the after-flight spectra are listed in Table 2.

The ratio of the thicknesses obtained before and after flight

for the two samples (viz., control and flight specimens) are

also given in the table. The numbers indicate that the

flight sample is approximately 40% thicker after flight,

which is attributed principally to the oxidation of the

silver in the atomic oxygen atmosphere.

RBS Results for Gold:

The RBS spectrum for the Au control and flight samples

before the flight are shown in Figs. 52 and 53. The width

of the tall peak on the right side of the figure can be noted

to be much greater than that for silver. This width is used

to deduce the thickness of the metal layer. These

thicknesses, which are listed in Table 2, are in the range of

5000 angstroms. The portion of the spectrum to the left in

the figure is again produced by the substrate, which in the

present case is also aluminum (cf. PIXE Results). The

spectra of the two samples can be noted to be essentially the

same at this point in time, namely, prior to the shuttle

flight. The corresponding spectra measured after the flight

are shown in Figs. 54 and 55. Notice that in this

particular case of gold the two spectra after the flight are

qualitatively the same as before flight. Furthermore, except

for the signal to noise ratio, which is determined by the

integration time and does not reflect any intrinsic property

of the samples, the spectra after the shuttle flight are

qualitatively no different than the spectra before the

flight. This contrasts markedly with the case of silver,

where the flight specimen manifested a quite different

appearance following exposure during flight. The conclusion

for gold, then, is that exposure to the atomic oxygen

atmosphere in low earth orbit produced almost no change

detectable by RBS. The thicknesses of the flight and control

samples obtained from the after-flight spectra are listed in

Table 2. The ratio of the thicknesses obtained before and

after flight for the two samples (viz., control and flight

specimens) are also given in this table. The numbers verify

that almost no change occurred during flight.
- 12 -

RBS Results for Palladium:

The RBS spectrum for the Pd control and flight samples

before the flight are shown in Figs. 56 and 57. The width

of the tall peak on the right side of the figure can be noted

to be much greater than that of most of the other samples.

This width yields thicknesses in the range of 6000 angstroms,

as can be noted from Table 2. The portion of the spectrum to

the left in the figure is again produced by the substrate,

which in the present case is again aluminum. The spectra of

the two samples can be noted to be essentially the same at

this point in time, namely, prior to the shuttle flight. The

corresponding spectra measured after the flight are shown in

Figs. 58 and 59. Notice that as in the case of gold, the

two spectra after the flight for palladium are qualitatively

the same as before flight. Furthermore, there are no

qualitative differences in the spectra which can be

attributed to the flight. Table 2 shows no thickness

differences produced by flight to within a precision better

than 5%. The conclusion for palladium, then, is the same as

that for gold, namely that exposure to the atomic oxygen

atmosphere in low earth orbit produced almost no change

detectable by RBS.

RBS Results for Platinum:

The RBS spectrum for the Pt control and flight samples

before the flight are shown in Figs. 60 and 61. The width

of the tall peak on the right side of the figure is not very

large, and this is reflected in the sample thicknesses

deduced (viz., approximately 500 angstroms). (These

thicknesses are listed in table 2.) The substrate is again

aluminum. The spectra of the two samples can be noted to be

essentially the same. The corresponding spectra measured

after the flight are shown in Figs. 62 and 63. Notice that,

as in the case of gold, the two spectra after the flight are

qualitatively the same as before flight, except for the

irrelevant matter of the difference in the signal to noise

ratios because of the different integration times. As

contrasted to the case of gold, however, there is an increase

in the measured thickness of the flight sample relative to

the control sample: Whereas the ratio of the thickness of

the two samples (flight to control) prior to flight was

1.002, the corresponding ratio after flight was found to be

1.211. (See Table 2.) The conclusion is that the atomic

oxygen atmosphere in low earth orbit produced a change in the

platinum sample thickness which was detectable by RBS. The

PIXE data also lead to this same conclusion.
- 13 -

RBS Results for Nickel:

The RBS spectrum for the Ni control and flight samples

before the flight are shown in Figs. 64 and 65. The width

of the tall peak on the right side of the figure gives the

sample thicknesses listed in Table 2. The thicknesses are in

the range of 2000 angstroms. The portion of the spectrum to

the left in the figure is again produced by the substrate,

which in the present case is again aluminum. The spectra of

the two samples can be noted to be essentially the same at

this point in time, namely, prior to the shuttle flight. The

corresponding spectra measured after the flight are shown in

Figs.- 66 and 67. Notice that two spectra after the flight

for palladium are qualitatively similar to those before

flight. However, careful examination indicates that there is

a qualitative difference in the region of the spectrum to the

left (i.e., the substrate produced portion) which can be

attributed to the flight. Specifically, it can be noted that

the spectrum edge in the flight specimen is more rounded

after flight that that of the control specimen, which

indicates an interdiffusion at the interface. Table 2 shows

no thickness differences produced by flight to within a

precision better than 5%. Note also from Fig. 67 for the

flight specimen after flight that there is a bump in the

spectrum between the Ni and the substrate portions. This

indicates some element in the Cr, Mn, Fe weight range lighter

than nickel is present on the surface of the flight sample

which is not on the control specimen. This conclusion is

confirmed by the PIXE data.

RBS Results for Copper:

The RBS spectrum for the Cu control and flight samples

before the flight are shown in Figs. 68 and 69. The widths

of each small peak on the right side of the figure is used to

deduce the thickness of the metal layers. The thicknesses,

as listed' in Table 2, are of the order of 2000 angstroms.

The substrate is again aluminum. The spectra of the two

samples can be noted to be essentially the same. The

corresponding spectra measured after the flight are shown in

Figs. 70 and 71. Notice that the two spectra after the

flight are qualitatively the same as before flight.

Furthermore, except for the signal to noise ratio, the

spectra after the shuttle flight are qualitatively no

different than the spectra before the flight. Table 2 shows

that within 5% precision there is no change in the thickness

produced by flight. As for the case of gold, the conclusion

is that exposure to the atomic oxygen atmosphere in low earth

orbit produced almost no change detectable by RBS. This was

an unexpected finding, because visually the flight sample

looked darker than the control sample after flight (cf.

Visual Observations Section).
- 14 -

RBS Results for Aluminum:

The RBS results for aluminum were not as definitive as

for the other metals, as can be appreciated by looking at the

spectra before flight (Figs. 72 and 73) and after flight

(Figs. 74 and 75). Because the peaks are not well

pronounced, there was great difficulty in obtain good

estimates for the sample thickness. The source of the

difficulty was the substrate material, namely stainless

steel, which is heavier than aluminum so that the Al peak is

superimposed on the substrate spectrum. From Table 2, it can

be noted that no definitive thicknesses were obtained before

flight, whereas the data taken after the flight gave

thicknesses in the 1100 to 1300 angstrom range. There were

no qualitative differences, apart from signal to noise ratio,

to be noted in the spectra of the two samples taken before

and after flight.

RBS Results for Chromium:

Figures 76 and 77 illustrate the RBS data for Cr for the

control and flight specimens before flight. Qualitatively

there is no difference to be noted in the spectra. The

thicknesses as listed in Table 2 are in the range of 800

angstroms. Figures 78 and 79 show the corresponding spectra

after the flight. Qualitatively there are no differences to

be noted in the portion of the spectrum due to the chromium

but note from Fig. 79 that there is a bump on the substrate

portion of the spectrum for the flight sample. This

indicates that the flight sample has an oxygen concentration

which is not present in the control sample. This is most

likely in the form of an oxide greater than 100 angstroms in

thickness on the surface of the chromium. Although both the

flight specimen and the control specimen appear to have

decreased in thickness over the period of time spanning the

flight, but with such thin metal films, it is difficult to

access whether this is a real effect or simply due to lack of

precision in the measurements.
- 15 -

PROTON-INDUCED X-RAY EMISSION

Introduction

The objectives of the PIXE measurements were to provide

an independent confirmation of the specimen elemental metal,

to ascertain the major impurity metals, and to see what trace

impurities are present on the sample surfaces after the

flight. In particular it was considered likely that the

trace impurities on the surface might be different for the

flight and control specimens due to the chemical reactions

with atomic oxygen which were possible for the flight

specimens.

The primary PIXE data are given in Figs. 80 through 95.

The trace metals indicated by the spectra are indicated on

each figure in question, and a summary of the results for

each metal specimen is given in the discussion below. The

conclusions to be reached are that the evaporated metal films

did contain significant impurity metal concentrations, and

there were differences in the trace impurities on the sample

surfaces depending upon whether or not the sample was a

flight or a control sample. The amount of information

obtained is large in volume and varied in nature, so the

reader is invited to extract the particular information which

has a bearing on his particular question at the moment.

Shown in Fig. 96 is the Iron 55 calibration curve

utilized in the data analysis.

Experimental Results

PIXE Results for Silver:

The x-ray spectrum for the Ag control sample is shown in

Fig. 80 and that for the corresponding flight sample is

shown in Fig. 81. Impurities to be noted from the spectrum

are Si and Mn. The substrate material is primarily Al. The

ratio of the x-ray line intensity of the flight sample to

that of the control sample was found to be 1.21, which is

indicative of the relative number of Ag atoms in these two

metal films. The conclusion is that the flight sample has

more Ag than the control sample. This is in qualitative

agreement with the RBS results, which gave 1.42 as the

corresponding ratio.
- 16 -

PIXE Results for Gold:

The x-ray spectrum for the Au control sample is shown in

Fig. 82 and that for the corresponding flight sample is

shown in Fig. 83. The substrate material is primarily Al.

The ratio of the x-ray line intensity of the flight sample to

that of the control sample was found to be 1.05. The

conclusion is that, within experimental error, the flight

sample has approximately the same amount of Au as the control

sample.

.PIXE Results for Palladium:

The x-ray spectrum for the Pd control sample is shown in

Fig. 84 and that for the corresponding flight sample is

shown in Fig. 85. The one impurity to be noted from the

spectrum is Cr. The substrate material is primarily Al. The

ratio of the x-ray line intensity' of the flight sample to

that of the control sample was approximately 1, indicating

that the flight and control samples contained essentially the

same amounts of palladium. There were, however,

approximately 40% fewer Cr impurity atoms on the control

sample than on the flight sample.

PIXE Results for Platinum:

The x-ray spectrum for the Pt control sample is shown in

Fig. 86 and that for the Pt flight sample is shown in Fig.

87. The substrate material is primarily Al. The ratio of

the x-ray line intensity of the flight sample to that of the

control sample was found to be 1.14. The conclusion is that

the flight sample has more Pt than the control sample. This

is in qualitative agreement with the RBS results, which gave

1.21 as the corresponding ratio.

PIXE Results for Nickel:

The x-ray spectrum for the Ni control sample is shown in

Fig. 88 and that for the corresponding flight sample is

shown in Fig. 89. Impurities to be noted from the spectrum

are very low concentrations of Cr, Fe, and Mn. The substrate

material is primarily Al. The ratio of the x-ray line

intensity of the flight sample to that of the control sample

did not indicate any differences between the control and

flight specimens.
- 17 -

PIXE Results for Copper:

The x-ray spectrum for the Cu control sample is shown in

Fig. 90 and that for the Cu flight sample is shown in Fig.

91. Impurities to be noted from the spectrum are Si, S, Cr,

Fe, and Ni. The substrate material is primarily Al. The

ratio of the x-ray line intensity of the flight sample to

that of the control sample was found to be approximately 1,

so the flight sample had the same number of Cu atoms as the

control sample.

PIXE Results for Aluminum:

The x-ray spectrum for the Al control sample is shown in

Fig. 92 and that for the corresponding flight sample is

shown in Fig. 93. Impurities to be noted from the spectrum

are S, Cr, Fe, and Ni. The substrate material is stainless

steel. The ratio of the x-ray line intensity of the flight

sample to that of the control sample was found to be 0.85,

which indicates that the flight sample has fewer Cr atoms

than the control sample. The Cr, Fe, and Ni concentrations

were the same for the flight and control samples, which is to

be expected since the substrate is stainless steel. The S

concentration was lower by 15% in the flight sample, the same

as the difference in the amount of Al in the two films.

PIXE Results for Chromium:

The x-ray spectrum for the Cr control sample is shown in

Fig. 94 and that for the corresponding flight sample is

shown in Fig. 95. The substrate material is primarily Al.

The ratio of the x-ray line intensity of the flight sample to

that of the control sample was found to be 1.07, indicating

that the flight sample had somewhat more Cr atoms that the

control sp'ecimen. An impurity to be noted from the spectrum

is Cu, which decreased by about 15% for the flight specimen

relative to the control specimen.

Comments:

It may be noted that the spectra for the flight and

control specimens of a given metal often have a different

signal to noise ratio. This is not due to any fundamental

difference in the two specimens, but instead is to the fact

that the exposure time to the proton beam was notexactly the

same for the two. This was taken into account in the

normalization process in reducing the data. Probably this

does lead to some greater uncertainty in the results than

might be the case had the exposure times been chosen to be

exactly the same.
- 18 -''

The depth of the sample region probed is also of

interest when studying the data. The fall-off distance of

the proton beam in the silver specimens, for example, is

estimated to be approximately 1000 angstroms.

It should be noted that PIXE does not detect the

extremely light mass elements, such as carbon, oxygen, and

fluorine. It may be safely said that no elements lighter

than fluorine appear in the spectra.

RECOMMENDATIONS FOR FUTURE STUDIES

It is recommended that a series of measurements be

carried out on carefully prepared single crystals of copper,

silver and nickel of at least two crystal orientations. It

would be advisable to utilize at least three different

temperatures.
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Ag, Au, Pd, Pt, Ni, Cu, Al, Cr

Fig. 44
STS

_*

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c ^

0)

•1 / H0)

0

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c

O

'-M

Q.

0vj ^ 2.

to

1

n

1 7 Meta

evaporc

Specimens (before f

]ted on polished metal substrates

/

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IIIIIMMMlFITrr i T T I I I I i I I I I I I I I I I I I I I I I I I I I I I I I I I T I I I I I I I I I I I I

Ag, Au, Pd, Pt, Ni, Cu, Al, Cr

Fig. 45
0)

o

o

c

o

'+->

Q.

i_

o

(/)

_Q

STS—17 Metal Specimens (after flight)

evaporated on polished metal substrates

0

/

/

Al

Pd

Au

I I I I I I

'

*'

/ '

Cu

'

Jr

x

I I I I I I I I I I I I I I I I I I I I I I I I I I I I TT MIT I I I I I I I I I I I I I I I I I I I

Ag, Au, Pd, Pt, Ni, Cu, Al, Cr

Fig. 46
RUTHERFORD BACKSCATTERING

STS-17 Samples

Pd

6

0 I

Ji

a

!

i i ill

Au

Cu

Al

Thickness of Specimens B end A

Before Plifht K\l After Flight

Fig. 47
foft -

1500 L

<

o 1888

CO

io

o

588

8

8 288 480 600

CHANNEL NO.

800 1000

Fig. 48 Ag RRS Spectrum - Specimen A
606 I -

-J

UJ

2 1000

O

O

O

500

0

0 200 400 600

CHANNEL NO.

800 1000

Fig. 49 Ag RBS Spectrum - Specimen B
5000 -

4000

3000

2000

1000

0

0 100 200 300

__CHANNEL NO.

400 500

~c Fig. 50 Ag RBS Spectrum - Specimen C
_

UJ

o

o

o

8000

7000

6000

5000

4000

3000

2000

1000

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 51 Ag RBS Spectrum - Specimen F
1500 .

LJ

2

2

<

O

CO

hOi

O

5130

13

213(3 400 600

CHANNEL NO.

800 1000

Fig. 52 Au RBS Spectrum - Specimen A
2000 .

LU

O

CO

hO

O

1500 .

1000 .

S00

0

200 400 600

CHANNEL NO.

800 1000

Fig. 53 Au RBS Spectrum - Specimen B
6000 .

J

9

I

3

5 4000 .

3

0 100 200 300

CHANNEL NO.

400 500

Fig. 54 Au RBS Spectrum - Specimen C
111

z

z

7000

6000

Q 5000

CO

H

z

3 4000

O

3000

2000

1 000

0 i

0 100 200 300

CHANNEL NO.

400 500

Fig. 55 Au RBS Spectrum - Specimen F
UJ

o

CO

o 588

488 688

CHANNEL NO.

888 1888

Fig. 56 Pd RBS Spectrum - Specimen A
~ 6

-I

Id

500

CO

Io

o

0 200 400 600

CHANNEL NO. _.

800 1000

Fig. 57 Pd RBS Spectrum - Specimen B
4000 .

3000 .

2000 .

1000 _

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 58 Pd RBS Spectrum - Specimen C
4000 L

Ill

Z 3000

<

o

<0

HZ

O 2000

1000 .

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 59 Pd RBS Spectrum - Specimen F
, (o f! -

3500

LJ

2

2

CO

3000

2500

g 2000

o

1500

1125,00

500

0

0 200 400 600

CHANNEL NO.

600 1000

Fig. 60 Pt RBS Spectrum - Specimen A
o i -

3000

2500

o

CO

h2

O

O

2000

1500

1000

500

0

0 200 400 600

CHANNEL NO.

800 1000

Fig. 61 Pt RBS Spectrum - Specimen B
7000

6000

5000

4000

3000

2000

1000

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 62 Pt RBS Spectrum - Specimen C
14000 I

1 3000 '.

12000 "

_l

z 110001

x 10000"

o

05 9000 L

D 6000 I

o L

° 7000

6000 .

5000

4000

3000

2000 t

1000 '.

0

100 200 300

CHANNEL NO.

400 500

Fig. 63 Pt RBS Spectrum - Specimen F
V fo6l -

X

O

CO

ho

o

1000

Fig. 64 Ni RBS Spectrum - Specimen A
-$

1000

UJ

<

o

CO

h-z

o

0

 500

0

200 400 600

CHANNEL NO. \

800 1000

Fig. 65 Ni RBS Spectrum - Specimen B
1888

8

121 188 288 388

CHANNEL NO.

488 588

Fig. 66 Ni RBS Spectrum - Specimen C
8000 -

1000 .

0

200

CHANNEL NO.

400 500

Fig. 67 Ni RBS Spectrum - Specimen F
2888

LU

2

O

\

CO

Io

O

1580

288 488 688

CHANNEL NO.

888 1888

Fig. 68 Cu RBS Spectrum - Specimen A
1500

o

o

o

1000 -

S00

0

0 200 400 600

CHANNEL NO.

800 1000

Fig. 69 Cu RES Spectrum - Specimen B
5000 .

«

5 4000 _

%

3000 .

2000 _

1000 _

0

100 200 300

CHANNEL NO.

400 S00

Fig. 70 Cu RBS Spectrum - Specimen C
8000

7000

_J

UJ

z

< 6000

O

COI-z

O

O

5000 .

4000 .

3000 .

2000 .

t000 .

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 71 Cu RBS Spectrum - Specimen F
LU

O

CO

O

O

1000

500

0

0 200 400 600

CHANNEL NO.

800 1000

Fig. 72 Al RBS Spectrum - Specimen A
1580 .

UJ

z

<

o

CO

o

o

1000 _

500

400 600

CHANNEL NO.

800 1000

Fig. 73 Al RBS Spectrum - Specimen B
6000 -

5000 .

c

5

5 4000 .

3000 .

2000 .

1000 -

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 74 Al RBS Spectrum - Specimen C
20

0 300

CHANNEL NO.

400 50

0

Fig. 75 Al RBS Spectrum - Specimen F
c r - 1,11 ? - f\

LU

O

CO

O

O

500

0

0 200 400 600

__CHANNEL_NO

800 1000

Fig. 76 Cr RBS Spectrum - Specimen A
-

CO

§ 508

o

o

200 400 600

CHANNEL NO.

800 1000

Fig. 77 Cr RBS Spectrum - Specimen B
10

0 200 300

CHANNEL NO.

400 50

0

Fig. 78 Cr RBS Spectrum - Specimen C
512)00 .

u

z

I 4000

I

O !

CO

o

o

3000 .

2000 .

1000 .

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 79 Cr RBS Spectrum - Specimen F
28881

UJ

<

s

o

18881

(s)

00

8

I

8 288 388

CHANNEL NO.

488 588

Fig. 80 Ag PIXE Spectrum - Specimen C
UJ

<

o

o

o

0

0

o o •n 2

TJQ

O 2

o 3gF m

s

100 200 300

CHANNEL NO.

400 500

Fig. 81 Ag PIXE Spectrum - Specimen F
UJ

o

^v

i

8

8 188 288 388

CHANNEL NO.

488 588

Fig. 82 Au PIXE Spectrum - Specimen C
38000

tu

X 20000fe

H

O

O

0

u

»l

>0

If

t>

K

o

I

00

t

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so r0

c

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il 4

u

C r

) » <0 o

5 s

i '

Vn p*

0 100 200 300

JDHANNEL NO.

400 500

Fig. 83 Au PIXE Spectrum - Specimen F
8

o o•n

2o > 5

3) r2

«O =0

C Sa

> 63

8 188 588

Fig. 84 Pd PIXE Spectrum - Specimen C
Ul

o

18880

o

8

8 188 288 388

CHANNEL NO.

488 588

Fig. 85 Pd PIXE Spectrum - Specimen F
z

<

o

(0

o

o

10000

0

u

Ul

_)

»

_)

ac

0 100 200 300

CHANNEL NO.

400 500

Fig. 86 Pt PIXE Spectrum - Specimen C
48880

UJ

o

<0

ho

o

S

(V

f

v

0 , «•

~l

O

m

V^.

U

v>

j-

«i

r4

Oo

pi

100 2m 300

CHANNEL N0.__

500

Fig. 87 Pt PIXE Spectrum - Specimen F
Ill

o

o

48800

8

8 188 488 588

CHANNEL NO.

f Fig. 88 Ni PIXE Spectrum - Specimen C
IU

z

z

<

o

COI-z

o

o

-oil

O 2

O 33

-jg r-

,O "0

C. 23»

•<

0

100 200 300

CHANNEL NO.

400 500

Fig. 89 Ni PIXE Spectrum - Specimen F
Ill

u

0)

o £0888

488 588

CHANNEL NO.

Fig. 90 Cu PIXE Spectrum - Specimen C
IU

s

\

io

I J

TJ

O 2

O 5s

gs r-

«o -a

8 188 288 388

CHANNEL NO.

488 588

Fig. 91 Cu PIXE Spectrum - Specimen F
120001

u

z

z

o

CO

z

o

o

40000

0

0

14

•£ y

r i c i *

§

V, «

•**v J

100 200 300

CHANNEL NO.

400 500

Fig. 92 SA1 PIX E Spectrum - Specimen C
Id

O

8

0

0 100 200 300

CHANNEL NO.

400 500

Fig. 93 Al PIXE Spectrum - Specimen F
Ul

o

z

oo

30000 21

18888 o\l

N

rt

8

'

 s 1 It •>

Q tS 1 I!

* Ifel 1 II ^

•"I I 1 11 °° ^o

*» JM 1 II > £

^11 V,. l\

yv,/ \« — ^ — rv>_ / V/\_ t yv • i t t t i

8 188 288 888

CHANNEL N

Fig. 94 Cr PIXE Spectrum'-" Specimen C

588
UJ

\

CO

10000

0

0 100

s

V

<J

I

s

200 300

_CHANNEL NO.

400 500

Fig. 95 Cr PIXE Spectrum - Specimen F
1

-1

LU

Z

Z

0 12000

CO

1-

z

D

O

0

6000

4000

0^^

0

•

•

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u

K

„ X

sX

II

k

{j

j r. ^

ST ct.)r>iM.il-'''vo^*

09

^ ^ r \

i ck ^

g c. W X-V V,

la - o. do { 9 %ff&7

d| = 0.dl77«?l7<3S

J

^

S

T -V77 39.^V^5'0

jy ^'fi ',7^r7*

f

 7-9/77 tf7.1f75

^ rf _ , ,. -. -

o*!* Y tlY'fZ.tre

o J.OV-7 ^iJ.^VtfV

to ?» 9tf V <U? 5". T 75*5*

N

•^. y/V I'll" BtfO

^

M

k

\

1 1 H ** * ? ' I ' I 1 *

100 200 300 400 500

CHANNEL NO.

Fig. 96 Iron Calibration PIXE Spectrum
Table 1

ELLIPSOMETER DATA ON EVAPORATED METALS

Specimen,

Thickness (nominal),

Data Point, Before Flight After Flight

& the Substrate n k n k

Ag (2000 A)

on 6061 T6 Al

Au (5000 A)

on 6061 T6 Al

Pd (5000 A)

on 6061 T6 Al

Pt (500 A)

on 6061 T6 Al

Ni (2000 A)

on 6061 T6 Al

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

—

0.5107

0.5142

0.5067

0.5071

0.2361

0.2363

0.2458

0.2442

0.4955

0.4951

0.4800

0.4818

0.4999

0.5004

0.4971

0.4987

1.6781

1.6815

1.6816

1.6756

1.6368

1.6392

1.6406

1.6408

2.2334

2.2424

2.2261

2.2273

2.1611

2.1600

2.1278

2.1253

1.8451

1.8460

1.8748

1.8759

1.8350

1.8350

1.8310

1.8289

3.2876

3.2885

3.2629

3.2644

3.5285

3.5303

3.5206

3.5225

2.4255

2.4191

2.3873

2.3858

2.4440

2.4461

2.4370

2.4388

3.2789

3.2827

3.2459

3.2446

3.1840

3.1841

3.1653

3.1630

2.6452

2.6427

2.6414

2.6420

3.2019

3.2035

3.2276

3.2281

2.8488

2.8455

2.8692

2.8701

2.8343

2.8322

2.8944

2.8968

0.2907

0.2874

0.2857

0.2823

1.9270

1.9307

1.9319

1.9308

0.5025

0.5041

0.5024

0.5014

0.5615

0.5630

0.5352

0.5360

1.6877

1.6890

1.6976

1.7186

1.4505

1.4478

1.4373

1.4334

2.1549

2.1549

2.1577

2.1581

1.8115

1.8103

1.8162

1.8091

1.7183

1.7215

1.7150

1.7192

1.8177

1.8162

1.8229

1.8236

3.1972

3.1946

3.2054

3.2028

1.5010

1.4958

1.4963

1.4939

2.3958

2.3976

2.3820

2.3822

2.2713

2.2729

2.2144

2.2172

3.1213

3.1201

3.1339

3.1605

2.8146

2.8203

2.8030

2.8028

2.6887

2.6832

2.6866

2.6887

3.1422

3.1434

3.1538

3.1519

2.9088

2.9097

2.9165

2.9183

2.2375

2.2379

2.2426

2.2417
Table 1 (continued)

ELLIPSOMETER DATA ON EVAPORATED METALS

Specimen,

Thickness (nominal),

Data Point, Before Flight After Flight

& the Substrate n k n k

Cu (2000 A)

on 303 stainless

steel

Al (500 A)

on 303 stainless

steel

Cr (500 A)

on 2219-T87 Al

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

A. la

A.lb

A.2a

A.2b

B.la

B.lb

B.2a

B.2b

0.9028

0.9033

0.9280

0.9269

0.9468

0.9510

0.9509

0.9509

0.9953

1.0139

1.0053

1.0054

1.0007

1.0052

0.9894

0.9972

2.9355

2.9300

2.9406

2.9469

2.9232

2.9322

2.9237

2.9168

2.5370

2.5381

2.5715

2.5720

2.5995

2.6000

2.6052

2.6052

5.6940

5.7003

5.6867

5.6744

5.3867

5.3889

5.3312

5.3322

2.9470

2.9457

2.9330

2.9388

2.9506

2.9527

2.9486

2.9534

0.9379

0.9378

0.9331

0.9327

0.6282

0.6363

0.7431

0.7415

1.6199

1.6246

1.4739

1.6275

1.4225

1.4261

1.4139

1.4117

2.7999

2.8037

2.8191

2.8252

2.4469

2.4392

2.4344

2.4338

2.3463

2.3486

2.3487

2.3477

1.8977

1.9071

1.9822

2.0117

5.1394

5.1405

4.8619

5.1387

4.3317

4.3325

4.3221

4.3234

3.1743

3.1756

3.1669

3.1551

2.5845

2.5851

2.5781

2.5796
Table 2

RUTHERFORD BACKSCATTERING DATA

Before After

Metal Flight Flight

Specimen L (A) L (A) B/A F/C

Ag

Mi

Pd

Cu

Au

Cr

Pt

rat 1 j.

| —

B 2325 F

A 2325 C

B 1931 F

A 1951 C

B 6401 F

A 6342 C

B 2033 F

A 2115 C

B 4994 F

A 5254 C

B 895 F

A 870 C

B 530 F

A 529 C

B

_

A

3214

2268

1906

1986

6368

6513

2107

2130

5173

5310

814

766

799

660

1±Y flQ^ J y 3

1277

1.00

0.99

1.01

0.96

0.95

•

1.03

1.00

1.42

0.96

0.98

0.99

0.97

1.06

1.21