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I D-R13 418 DSC ELECTRICAL CONDUCTIVITY AND NR STUDIES OF SALT 1
I PRECIPITATION IN PPO C.. (U) HUNTER COLL NEW OR DEPTUN OF PHYSICS AND ASTRONOMY J J FONTANELLR ET AL.
WLRSIID tJUL 9? TR-27 N"14-8-F-0OSS1 F/G ?/4 U
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MICROCOPY RESOLUTION TEST CHARTNATIONAL BUREAU OF STANDARDS- 1963-A
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O~iCFILE COEY
OFFICE OF NAVAL RESEARCH
Contract NOOO14-87-AF-O0001
R&T Code 413d001--02
Technical Report No. 27
DSC, Electrical Conductivity, and NMR Studies ofSalt Precipitation in PPO Complexes
by
John J. Fontanella & Mary C. Wintersgill
Prepared for Publication
in the
British Polymer Journal
U. S. Naval Academy D T ICDepartment of Physics ELECTE
Annapolis, MD 21402-5026
July 1, 1987 U
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11. TITLE (include Security Classification)
DSC, Electrical Conductivity, and NMR Studies of Salt Precipitation in PPO Complexes(Uncl ass if ied)
12. PERSONAL AUTHOR(S) John J. Fontanella and Mary C. Wintersgill
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.... DSC- nd electrical cofiductivity measurements of PPO complexed with 9 and
(KCN'are reported. - In addition, 23 NMR measurements of PPO8NaI, both at ambient and7elevated pressure (2.0 kbar) have been performed. The DSC data clearly yjidicate that
the salt precipitates out of the complexes at about 850"for NaI and 600 for KSCN.
1 These effects are manifested by a dramatic departure of the conductivity from VTF
behavior, and a relatively shArp drop in mobile Na conqptration deduced from NMRmeasurements at somewhat elevated temerature (about 805t). High pressure NMR
linewidth measurements are consistent with a pressure-induced increase in the glass
transition temperature.
114 c
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John J. Fontanella 301-267-3487n's rf 10 R1 AI 77 . . . .
DSC, Electrical Conductivity, and NMR Studies
of Salt Precipitation Effects in PPO Complexes
Mary C. Wintersgill and John J. Fontanella
Physics DepartmentU.S Naval Academy
Annapolis, MD 21402 U.S.A
Steven G. Greenbaum and Kregimir J. Adamid
Physics DepartmentHunter Colle e of CUNY
New York, NY 10021 U.S.A.
Keywords: ion-conducting po ymer; salt precipitation; NMR; DSC;poly(propylene oxiae)
Aoession For
NTIS GRA&IDTIC TABUnannounoed 0
Justifioation ,
Distribution/Avallabillty Codes
iAvail and/orDist specal
SYNOPSIS
DSC and electrical conductivity measurements of PPO complexed
with Nal and KSCN are reported. In addition, 23Na NMR measurements
of PPOsNaI, both at ambient and elevated pressure (2.0 kbar) have
been performed. The DSC data clearly indicate that the salt preci-
pitates out of the complexes at about 850C for Nal and 600C for
KSCN. These effects are manifested by a dramatic departure of the
conductivity from VTF behaviour, and a relatively sharp drop in
mobile Na concentration deduced from NMR measurements at somewhat
elevated temperature (- 800C). High pressure NMR linewidth measu-
rements are consistent with a pressure-induced increase in glass
transition temperature.
2
INTRODUCTION
Poly(propylene oxide) (PPO) is known to form amorphous ion con-ducting complexes with alkali metal salts.-I-3 Previous studies of
PPO complexed with LiClO42 and NaClO 43 have shown that large scale
segmental motion of the polymer chains is principally responsible
for ionic transport, in general agreement with the results of a wide
array of recent investigations. The studies in our laboratories2 ,3
can be summarized briefly as follows. The electrical conductivitytemperature dependence is best described by a VTF-type relation4
0' = A T-1 / 2 exp[-Ea/k(T - To)) (1)
where Ea is the apparent activation energy and To is the temperature rof "zero configurational entropy", about 40-50 K below the glasstransition temperature, Tg. The temperature dependence of theelectrical relaxation time associated with the -relaxation which
governs the glass to rubber transition in pure PPO can be described
in an analogous manner. It has been shown that the activationenergies for conductivity in the complexes and electrical relaxation
in pure PPO are the same when one takes into account the differentTo values associated with each material. Similarly, activationvolumes for conductivity derived from variable pressure data in the
complexes and the -relaxation in PPO were shown to be the same ina given temperature interval relative to To .
23Na NMR studies in PPO8NaClO 4 have shown that: (1) generation
of mobile ions is a weakly thermally activated process that accountsfor only a minor contribution to the overall conductivity; (2) NMRsignals associated with the mobile fraction of Na ions exhibitmotional line-narrowing beginning in a small temperature interval
above Tgo These results, taken together, demonstrate the importanceof polymer chain mobility to ion transport, in general agreement
with a wide array of recent investigations.
The present study concerns related work on PPO:NaI and PPO:KSCNcomplexes. In particular, it is observed that these materials
. .IL '
exhibit behaviour similar to that of previously investigated PPOcomplexes, however they become unstable at moderate temperatures
(<1000 C). As will be discussed, the instability is manifestedultimately by the separation of the salt from the polymer.
We have performed differential scanning calorimetry (DSC),
electrical conductivity and 23Na nuclear magnetic resonance (NMR)
measurements on PPOsNaI. The NMR measurements were performed both at
ambient pressure and at applied hydrostatic pressure up to 2 kbar
(0.2 GPa). In addition, DSC and conductivity data for PPOsKSCN are
presented.
EXPERIMENTAL
The host material studied was Parel 58 (Hercules, Inc.)
elastomer which is a sulfur-vulcanizable copolymer of propylene
oxide and allyl glycidyl ether. As the primary constituent is
propylene oxide, the material will be referred to throughout thispaper as PPO. The samples were prepared by solution casting using
anhydrous methanol as the solvent and commercially obtained NaI,which was heated at 100C in a vacuum oven overnight, as the salt.
All procedures including loading of the samples into the varioussample holders were carried out in a dry box; the sample for the NMR
measurements was sealed in a glass tube under dry nitrogen. For the
high pressure measurements, the sample was loaded into the rf coil
in a N2 glove bag and then immersed in the pressure transmitting
fluid (3M - Fluorinert) contained in the pressure cell. The details
regarding the DSC, electrical conductivity and NMR equipment and
techniques are given elsewhere.2 ,3
RESULTS
The DSC results for PPOsNaI are shown in Fig. 1. Results foruncomplexed PPO are included for comparison. It is clear that the
complexed material is highly amorphous in that it exhibits a strongglass transition with a "central" Tg of about 60C. (The "onset" Tg
is about 0°C and the "end" is at about 120C.) Consequently, Tg isabout 680C higher than for the uncomplexed material for which the
"central" glass transition temperature is about -620C as shown in
Fig. 1c. An increase in Tg with the addition of salt to PPO is a
well known phenomenon
In addition, in the DSC studies for PPO8 NaI, a strong, sharp
endothermic event is observed at about 1000 C. In order to obtain
information concerning this feature, the material was annealed at
175 0 C, quenched to -140 0C as rapidly as possible in situ, and the
DSC studies repeated. Typical results for the quenched material -p
after annealing at temperatures above 140 0C are shown in Fig. lb. In p.
all cases, a strong glass transition typical of uncomplexed PPO is
observed. In addition, there is a high temperature exothermic event
followed by an endotherm. Similar behavior has been observed for
PPOaNaCIO4 where it was concluded that the high temperature
endotherm is due to the salt coming out of the polymer.3 The primary
evidence is that only the glass transition due to uncomplexed PPO is
observed after quenching from temperatures above that of the sharp
endotherm. Further, the material exhibits the original behavior
(Fig. la) after allowing the sample to sit at room temperature
overnight, i.e. the salt redissolves in the polymer. Salt
precipitation has been observed spectroscopically for PPO containing
NaSCN.5
In order to gain further evidence for this effect, electrical
conductivity studies were performed. (It was not possible to perform
such studies for PPOaNaCIO4 as the salt precipitation temperature
was outside the range of the conductivity apparatus.) The results
are shown in Fig. 2. It is seen that the electrical conductivity
begins to deviate from its lower temperature behavior at about 850C.
In order demonstrate this more quantitatively, the data in the
temperature range 280-355 K were analyzed with equation (1) with the
adjustable parameters A, Ea, and To . A non-linear least squares fit
of eq. (1) to the data was carried out and the results are Ea -0.093 eV, To - 199.3 K, and logl0A [$2-cm)-1 K1/2] - -1.1. The RMS
deviation in log100 was 0.008. These best-fit values are close to
these observed for other salts in PPO. However, they are not as
reliable due to the limited temperature range covered, and further,
the high temperature cut-off (where salt precipitation becomes
e5
important) is merely an estimate. In fact, the value for To is
about 80 K lower than the "central" Tg, which is a larger difference
than expected.
A general feature of the 23Na NMR results is the coexistence of
two separate lineshape components with substantially different spin-
lattice relaxation times (T1) and linewidths. As in previous studiesof similar complexes, the long-T1 and broad component is attributed
to bound Na species while the short-T1 and narrow component arises
from mobile Na+ ions.3 The ratio of the narrow line to broad lineintensities as a function of reciprocal temperature is plotted in
Fig. 3. That the difference between the lowest temperature value and
the maximum value (occurring just above room temperature) is onlyabout a factor of ten is indicative of the relatively minor rolethat "carrier generation" plays in the overall conductivity, which
changes by more than four orders of magnitude over the same
temperature range. The salt precipitation is manifested as a sharp
drop in mobile ion concentration above 800C.
Figure 4 is a plot of 23Na resonance linewidth (full width at
half maximum) as a function of temperature. The open symbols denotepartially saturated resonances which correspond to the mobile sodium
population. The solid symbols refer to the total (unsaturated)
linewidth. As in previous work3 , the linewidths of the mobile andbound Na's are nearly indistinguishable below Tg, only their T,values are distinct. It is clear from the data that motional
narrowing occurs above Tg, again in agreement with previous studies.
The increase in linewidth above - 600C is attributable to rapidspin-lattice relaxation (T1 - 300 1us) which introduces a lifetime
broadening contributions to the linewidth.
The application of hydrostatic pressure (up to several kbar)
has been shown to result in a decrease in conductivity of PPOcomplexes2'3 . In order to obtain a better understanding of the
mechanisms involved, we have performed some preliminary high
pressure NNR measurements. Figure 5 displays 23Na absorptionspectra (both lineshape components are present in each spectrum) at
- 400C, where motional narrowing effects are apparent. The bottom
spectrum corresponds to ambient pressure, while the top spectrum was'
acquired at 2.0 kbar (0.2 GPa). The effect of the applied pressure
is to broaden the resonance by about 25% to approximately the
linewidth of the sample at lower temperatures (below Tg). This
result is consistent with increases in To with pressure deduced fromconductivity measurements2 ,3. It is not presently known whether
these phenomena simply reflect the pressure dependence of Tg, or are
indicative of more subtle ion-polymer interactions. High pressureDSC measurements are currently underway in order to determine
directly the Tg pressure-dependence. Conductivity vs. pressure
studies, which may shed light on the salt precipitation process, are
also in progress.
Another example of this salt precipitation is evident uponviewing the data for PPOsKSCN, shown in Figs. 6 and 7. For this
material, the salt comes out of the polymer at a lower temperature,
about 600C as seen by a sharp endotherm at about 600C in Fig. 6.
That the material was complexed is shown by the single glass
transition temperature at about -250 C. Once again, upon thermal
treatment, the glass transition disappears with the appearance of an
uncomplexed PPO glass transition. This material is interesting
because the melting endotherms for the salt are at relatively low
temperature as shown in Fig. 6a. As shown in Figs. 6b and 6c,
similar endotherms are observed in the polymer after heating above
600 C. Since the salt precipitation occurs at a relatively low
temperature, the effect on the electrical conductivity is quite
dramatic as shown in Fig. 7.
CONCLUSIONS
PPO complexed with NaI has been shown to exhibit the same
general ion-conducting properties as other PPO-salt complexes at
lower temperatures, whereas salt precipitation effects are observed
in the former above - 850 C. The salt precipitation is manifested by
(i) a. relatively sharp endothermic "event" in the DSC, and
subsequent observation of a pure PPO glass transition (after
quenching); (ii) departure of the electrical conductivity from VTF-type behavior at elevated temperatures; (iii) a sharp drop in mobile
7
Na concentration, deduced from NMR measurements, above - 800C. PPO"
complexed with KSCN exhibits even more dramatic salt precipitationeffects, as evidenced by corresponding features in the DSC and
conductivity data occuring at a lower temperature (- 600C) as wellas observation of KSCN melting endotherms in the complex.
Preliminary NMR measurements on PPOsNaI at an applied hydrostaticpressure of 2.0 kbar (0.2 GPa) are consistent with a pressure-
induced increase in Tg.
ACKNOWLEDGMENTS
The authors would like to thank Hercules, Inc. for supplying
the Parel 58 elastomer. The assistance of Ms. Meng Chiao, Ms.
Gillian Reynolds, and Mr. Yiu Sun Pak with the NMR measurements and
lata analysis is gratefully acknowledged. This work was supported
in part by the Office of Naval Research and the PSC-CUNY Research
Award Program.
REFERENCES
1) Armand M.,Chabagno M., and Duclot M.J.; in: Fast Ion Transportin Solids, eds.Vashishta P. Mundy J.N., and Shenoy G.K.(North-Holland, Amsterdam, 1479), p. 131.
2) Fontanella J.J., Wintersgill M.C., Smith M.K., Semancik J., andAndeen C.G.; J. Appl. Phys., 1986, 60, 2665.
3) Greenbaum S.G., Pak Y.S., Wintersgill M C Fontanella J.J.,Schultz J.W., and Andeen C.G.; J. ElectrocAem. Soc., in press.
4) Vogel, H., Physik Z., 1921, 22, 645; Tammann, V.G. and Hesse,Anorg. Allg. Chem, 1926, iBT, 245; Fulcher, G.S., J.Am.
Ceram. Soc., 1925, 8, 339.
5) Teeters D. and Frech R.; Solid State Ionics, 1986, 18&19, 271.
8
FIGURE CAPTIONS
Figure 1. DSC plot for a) uncomplexed PPO, b) as prepared PPO8NaI,
and c) PPO8NaI after having been annealed at 175 0 C and
quenched, in situ, to -140 0 C. Scanning rate is 10 K/min.
Figure 2. Arrhenius plot of the electrical conductivity data for
PPO8NaI. The squares correspond to the data and the solid
line is the best fit VTF equation (equation 1).
Figure 3. Arrhenius plot of 23Na narrow to broad line intensity
ratios in PPOsNaI.
Figure 4. 23Na linewidth in PPOsNaI. The solid symbols denote the8p
total linewidth while the open symbols refer to partially
saturated resonances, reflecting the presence of only the
mobile sodium population.
Figure 5. 23Na absorption spectrum in PPO 8NaI at 400 C. Bottom:
ambient pressure; Top: applied hydrostatic pressure of
2 kbar. (0.2 GPa) .
Figure 6. DSC plot for a) KSCN, b) PPO8KSCN, c) PPO 8KSCN after
having been annealed at 200 0 C and quenched, in situ, to
-140 0 C, d) uncomplexed PPO. Scanning rate is 10 K/min.
Figure 7. Arrhenius plot of the electrical conductivity data for
PPO8 KSCN. The solid line connects the data points.
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