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Using Electrolyte Flow as a Variable in Secondary Batteries

Stacey M. Watts
Chemistry Graduate Loyola College Chemistry Department

Dr. Robert B. Pond, Chair


Engineering Science Department of Loyola College 4501 North Charles Street Baltimore, Maryland 21210

Key Words Secondary Battery, Electrodes, Electrolyte, Power, Energy Prerequisite Knowledge General Chemistry, Electrochemistry Objective To determine the effect of electrolyte flow through a battery on voltage output Equipment and Materials Electrolytic Manganese (IV) Oxide, Graphite Solid Zinc Rod (1/2 diameter), Hack Saw KOH (40% by weight), Tap Water 400 mL Beakers Manufactured Graphite Electrodes, Nylon Stockings, Nylon Thread Delrin Separator PVC Pipe Battery Pack Voltmeter with Alligator Clips 5 Power Resistor Safety Precautions Manganese oxide is a known irritant to the eyes, skin, and respiratory system. Gloves and breathing masks should be worn when handling it. Potassium hydroxide can cause chemical burns; therefore, gloves should be worn when handling it.

Procedure Introduction Our main objective in this experiment was to determine the effect of electrolyte flow through a secondary battery. In order to do this, the zinc-manganese oxide system was chosen because it was 1) safer to use than a lead-acid battery system and 2) because literature tells that the system is rechargeable for a limited number of uses.

Preliminary Preparations The battery pack was designed and assembled for testing. The plates were made in the following manner: a graphite rod (2.2 in diameter) was manufactured on a lathe from a solid rod of nuclear grade, high density graphite. Discs were then cut with a band saw (3/16 thick). A square hole pattern was created on a computer (Figure 1) and then 1/8 holes were drilled into the discs using the computer layout and a table drill. The electrodes were loaded with active material in two different ways, depending on whether it was the cathode or the anode. The cathodic plate was painted with a paste consisting of 85 % manganese oxide and 15% graphite in tap water. For the anodic plate, fine zinc shavings were packed into the holes Figure 1. Electrode Layout using the end of a 1/8 drill bit. The zinc shavings were made by sawing away at a rod of solid zinc and then collecting the shavings in a beaker. Once the plates were made, conductor wires were attached to each plate using a screw connector (the wire was soldered to the screw and then shrink wrapped) in any one of the electrodes holes. Each plate was then placed into a nylon-stocking holder (actually the feet of pantyhose) and secured by tying nylon thread to close the tops of the nylon holders. The conductor wire was threaded through the top and bottom of the PVC pipe battery pack and the electrodes were placed in the battery pack with the Delrin

separator between them (Figure 2). The Delrin separator also was drilled with randomly spaced holes to allow flow of the electrolyte. The PVC pipe battery pack consisted of two parts (Figure 3): the top part, which was a two foot (2) long stand pipe that was glued into a standard PVC coupling; and the base, Figure 2. Electrode Assembly which was machined from a three inch

(3) OD solid block of PVC. The base also has a lip in it to contain the battery pack; the top part then screws into the base to encase the battery pack snugly. There is also a hole in the base to allow for electrolyte flow. Once the battery pack was assembled, the wires were connected to a voltmeter using alligator clips.

Testing Testing protocol was as follows: 1. A measured amount of KOH was poured into the battery pack. 2. Open voltage readings were taken every 15 or 30 seconds. Figure 3. Battery Pack Assembly
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3. Finally, the power resistor was connected to the battery and the voltages were recorded every 15 or 30 seconds. 4. Recharging was attempted by applying a reverse voltage to the battery for a certain amount of time. After a few minutes, the reverse voltage was discontinued and open voltage measurements were taken to see if recharging was successful. 5. As needed, KOH was repoured into the battery pack to ensure constant electrolyte flow by gravity. 6. After each series of runs, tap water was poured through the system to rinse off the electrodes and the electrodes were allowed to soak overnight in tap water. Upon returning to the disassembled battery pack, the electrodes were examined to see what physical changes had occurred to them.

Data

Details of Runs Maximum Voltage/Time Occurred 1.39 V/0 s 1.23 V/0 s 1.27 V/0 s 1.00 V/0 min

What's Being Tested 1 Open Voltage 2 Resistor Attached 3 a) Open Voltage b) Resistor Attached

c) Open Voltage d) Charging

e) Open Voltage

Length of Run Amount of KOH Poured 75 s 100 mL in beginning 300 s after 165 s, 100 mL added 5 min 200 mL in beginning 23 min 163 mL recovered from previous run and repoured; at 5 min, 150 mL recovered and repoured; at 13 min, 145 mL recovered and repoured; at 17 min, 145 mL recovered and repoured 12.5 min 150 mL recovered from previous 0.48 V/2-5.5 min run and repoured 11 min 162 mL recovered from previous 4.38 V/8 min run and repoured; at 6 min, 110 mL recovered and repoured 15 min 60 mL recovered from previous 0.222 V/15 min run and repoured

Table One. Summary of Tests

Voltage v. Time 1.5 Voltage (V) 1 0.5 0 0 100 Time (s) Graph One. Data from Runs #1 and #2 200 300

Run #1 Run #2

Voltage v. Time 5 Voltage (V) 4 3 2 1 0 0 10 20 30 40 50 60 70 80 Time (min) Graph Two. Data from Run #3 Note: The voltages in both graphs are absolute values of the voltage readings from the voltmeter. Open Voltage Resistor Open Voltage Charging Open Voltage Tap Water Rinse

Instructors Notes In order to theoretically determine how long the battery should run, we used Faradays Law: Moles Used in Reaction =
I *t n*F

where I is the total amps expended, t is the total time, n is the number of electrons transferred (in this case, n=1), and F is Faradays constant, 9.6458*104 C/mol. Zinc is the limiting reactant in our battery, therefore by plugging in the moles of zinc into the equation, we can solve for I*t, which will yield the maximum number of coulombs produced in the reaction. For Run #1 approximately 6 g of zinc shavings (65 g/mol) were packed into the electrode; if all the zinc was used in the reaction, 0.092 moles would have reacted. Solving for I*t gives 8904 C produced by the battery. In order to find out how long the battery should run, we used a simple proportion: we found our battery had created 150 C in 10 min; therefore 8,904 C would allow the battery to run for 594 min, or a little under 10 hours. This is theoretically how long the battery should have lasted. But by examining the data from all three runs, one can see this is not the case. So what caused the battery to under perform? One reason is that the battery could not hold a load. When the power resistor was attached the voltage dropped dramatically; in Run #3 the voltage dropped to 46% of what it was before the resistor was attached. Another reason is that there was loss of active material during the runs. One good thing about stationary electrolyte batteries is that loss of material is normally due to gravity. In our case, not only is gravity working against us but as the electrolyte washes through the battery it also takes with it some of the active material. This decreases the life of the battery since microscope findings of the zinc electrode show that only the exposed

surfaces of the zinc reacted in any way with the KOH. By digging deeper into the zinc, one could see that once the exposed surfaces were etched away, the inside still contained shiny zinc shavings. The zinc on the surface of the electrode was dull and gray. The biggest problem of the system was the fact that it was not rechargeable. By examining the data in Run #3 one can see that after a reverse voltage of about 4 V was applied for 11 min, the maximum voltage reached once the charging was completed was only 0.222 V (the readings taken after that are disregarded since tap water was poured through the system). In order to resolve the problems listed above, steps are being taken so that future studies produce more desirable results. One such step is the replacement of the Delrin spacer with a biological glass filter. The filter will only allow the electrolyte and any particle smaller than a few microns to pass through. This will help keep the active material from falling through the battery system. Another way in which we plan to keep the active material stationary is by replacing the graphite electrodes with electrodes of compacted active material. Discs would be made from compacted manganese oxide and graphite and also from compacted zinc. This would hopefully keep the material in place so that all of the material may be reacted, thereby increasing the life of the battery. We did accomplish the goal of making a flowing electrolyte battery. What we now have to focus on is refining the design of the battery so that we may increase battery life along with making the battery rechargeable.

Battery Pack Assembly Pictures

Picture One. Assembly Ready for Testing

Picture Two. Base of the Battery Pack Containing the Electrodes

Picture Four. Electrodes After Testing

Picture Three. Electrode Assembly

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Sources of Supplies/Equipment/Services Sigma-Aldrich: Manganese (IV) Oxide Fisher Scientific: KOH Pellets Johns Hopkins Machine Shop, Mr. Walter Krug: Solid Graphite Rod; Manufacturing of the PVC Pipe Battery Pack Loyola Machine Shop, Mr. Howard Moore: Hack Saw; Manufacturing of the Graphite Rod and Discs Loyola College Engineering Dept, Dr. Rob Pond, Jr.: Voltmeter; Graphite Powder; Zinc Rod; Beakers; Nylon Stockings; Delrin Separator; 5 Power Resistor; Use of Engineering Lab Stacey Watts: Nylon Thread

Acknowledgements I would like to thank Mr. Walter Krug, Mr. Howard Moore, and Ms. Janet Walszek (of the Loyola College Chemistry Dept.) for helping us get the supplies we needed to make our battery. I would also like to thank Dr. Rob Pond for being a wonderful teacher and lab partner.

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References Battery Council International. A Summary of Battery Chemistries. Online Posting. 2003. http://www.batterycouncil.org/different2.html Bode, Hans. Lead-Acid Batteries. Trans. by R.J. Brodd and Karl V. Kordesch. New York: John Wiley and Sons, 1977. Crompton, T.R. Lead-Acid Secondary Batteries; SLI (Automotive Batteries): Construction and Performance. Battery Reference Book. 2nd ed. Oxford: Butterworth-Heinemann, 1995. Dell, R.M. and D.A.J. Rand. Understanding Batteries. Cambridge: The Royal Society of Chemistry, 2001. Linden, David. Basic Concepts. Handbook of Batteries. 2nd ed. New York: McGrawHill, 1995. Scarr, Robert F. and James C. Hunter. Alkaline-Manganese Dioxide Cells. Handbook of Batteries. 2nd ed. New York: McGraw-Hill, 1995. Strem Chemicals. Material Safety Data Sheet for Manganese (IV) Oxide. Online Posting. 26 February 2001 http://www.strem.com/code/datasheets/251360.pdf

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