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https://ntrs.nasa.gov/search.jsp?R=19840026280 2020-05-20T17:25:49+00:00Z

(NASA-CR-171163) SURFACE ANALYSIS OF SPACE M84-34351SELZSCOPE MATERIAL SLICIRE&S douthly Report(Auburn Univ.) 70 p BC 104/RF A01 CSCI 034

unclasG3/69 24046

SURFACE ANALYSIS OF SPACE TELESCOPE MATERIAL SPECIMENS(NASS-35914)

Monthly Report for JL(1y(July 31 ,. 1984)

Albert Thomas Fromhold, Jr.Department o+ Physics

Auburn University. AL :36a49

IV-*. --c-0-4

oil

Prepared for

George C. Marshall Space Flight CenterMarshall Space Flight Center, Alabama 35812

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Abstract

Surface analysis by electron spectroscopy for chemicalanalysis (ESCA) was used to characterize a number of thesamples during the past month " With ESCAv the sample isirradiated with monoenergetic soft w~~ra^s and the resultingemitted electrons are energy anal/zed to determine thebinding energy of electrons to the surface atomz. The majorpeak were used in the quantitative determination

of the

surface composition. (Please refer to Tables 1 through 16which are interspersed with the figures.) The presence oftrace elements (impurities below 1% atomic composition) wasalso detailed. Initially a Survey scan was *'un for eachsample to deduce the elemental coii;position. Then the majorpeaks of interest and those of the trace elements wereindividually eXamined. After this, the samples were argonsputtered to etch away surface layers, and then additionalmeaSurements were carried out in order to obtain depthprofile information. Those species present only an thesurface could in this way be distinguished from those havinga significant depth distribution within the sample.

It was estimated on July ^^1 that the measurements were90% complete. It is expected that the measurements will be10o% complete by AUgUSt 710, 1984.

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ESCA Date for Silver and Copper Specimens

Silver

Four silver samples have thus far been examined: asilver interconnect flown on STS-8, a silver foil flown onSTS-B, the relevant control silver specimen for thesesamples, and a gold-plated silver foil which had beensubjected to the plasma asher for a period of two minutes"Several common trends were found for all silver samples:

t. The flight and ashed samples exhibited a slight decreasein binding energy (0"1 to 0 ° 3 eV) of the Ao 3d doubletrelative to the control. (These data are given in Figs. 1n2, 9, 21, and 22.) These results indicate an increase in thedegree of oxidation of

2. Chemical shifts toward oxygen species with lower O(Is)binding energies (B.E.) occurred in the flight and ashedsamples "(These data are given in Figs. 5 ,, 6, 11v 12 9 17918, 23» and 24)~

3. The control sample always had a Ag to O ratio of 1:1at the Surface of the sample. (These data are given inTables 2, 4, 6, and S. It should be pointed out, hpweverothat this is not necessarily evidence that the chemicalcomposition of the surface is AgO, although the data areconsistent with this interpretation.)

4. A decrease in carbon was observed in the awshed and flightsamples relative to the control. (See Tables &, 2r 3, 4, 5,6 ° 7, and B.)

The ashing processp surprising1y~ did not seem tosi0ulate very well the processes which occurred duringenposure to the ambient during flight. The flight samplesexhibited shifts toward increased surface concentrations ofoxygen at lower binding energies, but new chemical bondingforms were not observed. Figures 17, 18» 23, and 24 indicateonly shifts between oxygen species ori-ginally present on thesurface. On the other hand, the ashed samples exhibited notonly this effecto but enlscu the creation of new oxygen speciesat still lower binding energies (see Figs. 5, 6, 11 9 and12).

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Ashed and flight samples also differed in the silver tooxygen ratio. Whereas the control showed a i:l ratio, theashed samples showed a decrease and the flight samples showedan increase in this ratio. The results are as follows:

Silver-to-Oxygen Ratios

Control Sample: 1.0Gold-plated Silver after Ashing: 0.2Silver Fail after Ashing: 0.4Silver Foil after Flight: 2.5Silver Interconnect after Flight: 1.5

The gold-plated silver sample deserves special mentiondue to the unusual effect of the plasma asher treatment.Even the control, sample exhibited a silver peak at thesurface, whici is rather surprising. (It would be expectedthat the guld plating would have entirely protected the,underlying silver.) The ratio of gold to silver was found totie 4 to 1. After aching, gold was barely detectable (seeFigs. 3 and 4). Quantitatively it was found that the goldto silver- ratio went from 4 to 1 before ashing to a ratio of1 to 1.3 after asking. Possibly this could have been due to abulk: diffusion of the gold into the t;ilver foil duringa5hina. It seems unlikely that the gold was sputtered away,since the sample weight measurements by the Marshallpersonnel indicated no weight loss during ashing. Anotherpossible explanation is that the adhesion of the gold to thesilver w&s affected by plasma aching, so that the goldaggregated into small beads, thereby leaving the silversurface exposed.

The composition of the silver interconnect and theunderlying silver foil after flight were very similar (seeTables b and 8). However the control sample for theinterconnect was found to have a larger amount of graphiticcarbon. It was found that this carbon could be easilyremoved by sputtering. The flight interconnect had somewhatmore carbon than the flight f of 1 . The flight foil alsocontained sulfur hand chlorine, elements not not found on theinterconnect.

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Copper

Cupric oxide was 'FOUnd an both the control and -flightsamples (see Fig. 27). The amounts of carbon and oxygen wereless in the flight camp lesm as indicated below.

Oxygen-to-Copper and Carbon-to-Copper Ratios

O/CLI C/CU

Control Sample: 5.21 5.9Flight Sample: 1.1 3.8

A shift to lower binding energy oxygen was observed in theflight sample (see Fig. 28). The carbon type, howeverp wasunchanged (see Fig. 29).

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ESCA Data for Faint Specimens

Because the paint samples were non-mitallic, someelectrical charging occurred during the ESCA study. A's aconsequence, the positions of the peaks at times appeared asmuch as 6 eV higher than expected. This was more evident inthe A-276 and the 401-C10 specimens than in the Z-302specimen, the latter being scarcely affected by charging.The degree of surface charging depends nat only on the lowelectrical conductivity of the sample, but also on thethickness of the specimen because this will control the rateof charge leakage to the underlying metal substrate. Theconsequence is that peak positions were inconsistent fromsample to sample, and in addition, the peak; positions wereobserved to change with sputtering of the sample. Thereforethe energy axis of the ESCA scams should not be used to inferabsolute binding energy, and the shifts in energy should notbe used indiseriminantly to infer changes in chemicalbinding.

In view of the foregoing, it is not surprising that fewconsistent trends were found by means of ESCA for the paintspecimens. Nevertheless, the A-276 and Z-302 samples didshow a slight decrease in the silicon-to-oxygen ratio, whilethe 401-Clo sample exhibited a significant increase. Thedata supporting these statements are now given.

Silicon-to-Oxygen Ratios

A-276 Z-302 4C)1-CI':r

Control Sample: 0.48 0.29 0.13Flight Sample: 0.310 0.19 47.88

For the A-276 specimens, the silica, oxygen, and carbonpeaks were unaffected by flight, as indicated by comparisonof the flight and control sample data (see Figs. 31, 32, and3). For the Z-302 specimens, the silica peak was broader inthe flight sample, and the peak: was broadened by sputtering(see Figs. 34 and 35). No change occurred in the N(1s) or00s) peaks (see Figs. 36, 37, 40$ and 41) . Three forms ofcarbon were present on the Z- o2 control. The flight samplee;,hibited a shift in one of the higher binding energy formsof carbon (see Figs. 38 and 39).

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Although the peaks in the 401-C10 flight sample appearedto be shifted towards higher binding energy, this seems to be Va consequence of a difference in the degree of charging ofthe flight and control specimens. Perhaps the thicknesses ofthe samples were not the same. Assuming this to be the case,there does not appear to be a difference in the oxygenspecies between the flight and control specimens (see Figs.4: and 43). Two forms of silicon were present on the controlspecimen, with the higher binding energy form predominant.The flight sample, on the other hand, showed no lower bindingenergy form (see Figs. 44 and 45). The carbon peaksindicated a behavior resembling that of the Z -302 samples,namely, the flight sample exhibits a shift to a higherbinding form relative to the control sample (see Figs. 46and 47.

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