AD-A129 194 INCREASED ELECTROCHEMICAL WINDOW IN AMBIENT TEMPERATURE

NEUTRAL IONIC LIQ. . (U) STATE UNIV OF NEW VORK AT

BUFFALO DEPT OF CHENISTRV H LIPSZTAJN ET AL. JAN 84
UNCLASSIFIED SUNVBUF/DC/TR-15 N88814-79-C-8682 F/G 7/4 NL

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Increased Electrochemical Window in Ambient

Temperature Neutral Ionic Liquids
6 PERFORMING ORG. REPORT NUMBER

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7. AUTHORf«) 8 CONTRACT OR GRANT NUMBERf«.)

Marek Lipsztajn and Robert A. Osteryoung N00014-79-C-0682

CO
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Department of Chemistry
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'8 SUPPLEMENTARY NOTES

Prepared for publication in The Journal of the Electrochemical Society

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19 KEY WORDS (Continue on reverse eide if necessary «ncf identify by block number)

Molten Salts; Voltammetry; Neutral Melts

+
a.
CD
20 -ABSTRACT (Continue on reverie tide if necessary and Identify bv block number)

CO Arneutralf melt of exactly 1.0:1.0 mole composition of AlClJ.-RCl, where R+ is

«either N-(l-butyl) pyridinium or 1-methyl-3-ethyl imidazolium, has been shown to
have an increased electrochemical window of 3.5 and 4.5 V, respectively. System
characteristics are described.
-TV

DD ) j*üM7«. 1473 eOlTiON OF 1 NOV M IS OBSOLETE

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TECHNICAL REPORT NO. 15

INCREASED ELECTROCHEMICAL WINDOW IN AMBIENT TEMPERATUE NEUTRAL IONIC

LIQUIDS
by
rN-s
.v.*- Marek Lipsztajn and Robert A. Osteryoung

>u

Prepared for Publication in

Acce.-.^ion For
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January, 1984

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 K-^-WV *P •."rV*" ' • V UT -^ ;*i
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Increased Electrochemical Window in Ambient Temperature Neutral
fl
Ionic Liquids
M. Liputojn ond R. A. Osteryoung*
Department of Chemistry, State University of New York. Buffalo. New York 14214
In the past several years, low tempera-
ture molten salt systems composed of aluminum
chloride and alkylpyridinium salts have been
found (1-3) to be useful solvents for electro-
chemical and spectroscoplc studies of both
organic and Inorganic species. Recently
Wilkes et al (4) have developed a group of
dialkyl-imidazolium chloroaluminate melts
having a wider cathodic limit than the alkyl-
pyridinium chloroaluminates.
Both cathodic and anodic limits of these
solvents depend on the mole ratio of compon-
ents taken for the preparation of the molten
K I salt. for so-called basic melts
"AIM.3
(MC * * <1) the anodic limit corresponds
"RC1
to the electrooxidation of chloride ions and
is identical (5) for both N-n-butylpyridinium
chloride (BuPyCl)-AlCl3 and 1-methyl-3-ethyl-
imidazolium chloride (ImCl)-AlCl3 melts. The
cathodic limit for basic melts corresponds to
the electroreduction of the organic cation
(BuPy+ or Im+).
For acidic melts (MC > 1) the anodic and
cathodic limits are identical (5) for both
I chemical reactions, particularly those In-
RC1-A1C13 melts (R • BuPy+ or Im*) and corres-
pond to, respectively, tetrachloroaluminate
(A1CU") oxidation, to yield chlorine, and
heptachloroaluminate (AI2CI7") reduction, to
yield Al.
The electrochemical windows for these
melts measured at a tungsten electrode are shown
1n Figure 1.
The purpose of this communication is to
present the great advantage of use of a
neutral melt (MC • 1.00); preparation of this
melt consists of weighing appropriate amounts
of AlCls and RC1, and mixing. This roughly
neutral melt 1s subsequently adjusted by
addition of small amounts of either AlCls or
RC1 to obtain the proper electrochemical
window. As shown in Figure 1 the limits
established for neutral melts correspond to
anodic oxidation of A1CU" and cathodic
^Electrochemical Society Active Member
Key Words: Fused salts, depolarization,
discharge, voltammetry
1968
• ---• -f ,„ —<-*'* •*• *~ •'-1 - • '.V-V-V-V-V- .--'.-
Trrrr
reduction of R , giving a very wide electro-
chemical window (-v.3.6 V for 1:1 AlCls-BuPyCl
and ^4.4 V for 1:1 AlClj-ImCl melts
respectively). This extension of the
electrochemical window enables us to
investigate several redox systems inaccess-
ible for study 1n melts prepared by use of
an excess of basic (RC1) or addle (AlCls)
components. Some of these systems are of
fundamental importance in understanding the
chemistry of these melts.
As an example, the electrochemistry
obtained at a tungsten electrode 1n a 30 mmol
solution of BuPyCl 1n neutral AlClj-ImCl melt
1s presented in Figure 2. The quasi -
reversible oxidation of CT is observed (4)
as a discrete anodic voltammetrlc wave, while
cathodically the reduction of B'iPy* occurs.
More detailed studies of C1~ oxidation and
BuPy+ reduction will be presented In
subsequent publications; however it is worth
mentioning that this first process is con-
vective diffusion controlled at a rotating
disc electrode and that the CT oxidation
wave can be very useful 1n studies of many
volving chloride complexation with a metal
ion.
In a melt symmetric to that discussed
above (i.e. a neutral melt with a small ex-
cess of AICI3 added (6)) the convective -
diffusion controlled reduction of A12C17* at
a rotating disc electrode 1s observed and
this wave can be also very useful.
The very wide electrochemical window of
neutral A1C13-RC1 melts appears very promis-
ing from the point of view of use as a
solvent for new high energy density
batteries. Applicability of this system to
studies Involving redox and conducting
polymeric electrodes is in progress (7).
 '."•" '-."•".••" "•"."-" "•" '•" »•% ;v. I1, i'i.ii*) :•'.•'.• .V ' • ." .• .", .<. , j' r . w ..i

M VoL 230, No. 9 INCREASED ELECTROCHEMICAL WINDOW 1969

M
:i ACKNOWLEDGMENT

This work was supported 1n part by the

Air Force Office of Scientific Research and
the Office of Naval Research.

This paper was presented 1n part at the

4th International Symposium on Molten Salts,
the Electrochemical Society Meeting, San
Francisco, May 1983.
Manuscript «uteittad Am* «, 1963.

J £5 ' T5 ' So
E vi Al Al «ml in 1.51 AICI3 ImCI Nell
' ^To •tx>
REFERENCES

1. H. L. Chum, V. R. Koch, I. L. Miller and

K. A. Osteryoung, J. Amer. Chem. Soc,
97, 3264 (1975).
2. X* Robinson and R. A. Osteryoung, ibid,
101, 323 (1979).
Cyclic voltammetric curves recorded on 3. R. J. Gale and R. A. Osteryoung, Inorg.
tungsten electrode (area 0.0784 cm2) 1n Chem., 18, 1603 (1979).
(a) basic AlCl3-ImCl melt (MC * 0.67) 4. J. S. WiTkes, J. A. Levlsky, R. A. Wilson
(b) acidic AlClj-ImCl melt (MC - 1.2) and C. L. Hussey, ibid., 2JL, 1263 (1982).
(c) neutral A1C1 >-I^iCl melt (MC « 1.00) 5. Z. Karoinski and R. A. Osteryoung, in
(d) neutral AlCl3-BuPyCl melt (MC • 1.00) preparation.
Sweep rate • 0.05 V s"1, temperature • J. Robinson and R. A. Osteryoung, This
30° C. Journal, 127, 122 (1980).
7. P. G. Pickup and R. A. Osteryoung, This
Journal, submitted for publication.
4

120«. A

^lO" IT" -LO

E vt AI/AI (III) in 1.5:1 Al CI3 ImCI Melt

Cyclic voltammetric curve recorded on

tungsten electrode (area 0.0784 cm*) at
30°C in 30 mmol solution of N-n-butyl-
pyridinium chloride in neutral AlClj-ImCl
melt (MC * .994), sweep rate 0.05 V s"1.

,-\".\
i-i-i . <Jf m,, i^V -•/_. V A. .N Al
 ••HPii ••. f'-'T?".' ?; !• .• .» •••.•'.I *J»*»*.'' ':'*^'5'.T''-'J'>'.''.',)','''^;

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Jackson State University Brown University
Jackson, Mississippi 39217 Providence, Rhode Island 02192

Dr. Theodore Beck Dr. C. A. Angell

Electrochemical Technology Corp. Department of Chemistry
3935 Leary Way N.W. Purdue University
Seattle, Washington 98107 West Lafayette, Indiana 47907

Dr. Farrell Lytle Dr. Thomas Davis

Boeing Engineering and Polymer Science and Standards
Construction Engineers Division
P.O. Box 3707 National Bureau of Standards
Seattle, Washington 98124 Washington, D.C. 20234

Dr. Robert Gotscholl

U.S. Department of Energy
MS G-226
Washington, D.C. 20545

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