Badger ElectrochemistsGiddings Award Symposium
Leslie J. Lyons
Department of Chemistry
Grinnell College
Grinnell, Iowa 50112
CongratulationsAlanah!
Outline
• Badger Electrochemists (1952 - present)
• Analytical Chemistry at Grinnell– Teaching: Introductory and Advanced– Research: Silicon Electrolytes for Lithium Battery
Applications
• Acknowledgements
Badger Electrochemistry Home
This photograph, from 1978, shows the Daniels building from the northeast, on the corner of University Avenue and Mills Street. Photo courtesy of UW-Madison University Communications.
Irving ShainPhotos courtesy of UW-Madison University Communications.
Shain Chemistry Research Tower
The Shain Tower Dedication
Primitive cyclic voltammetry in 1963.
Photos courtesy of Irving Shain and UW Dept. of Chemistry
Students in the laboratory in 1962 (L to R): R. Nicholson, B. Schwarz, B. K. Hovsepiar, and D. Polcyn
NanoBucky
http://hamers.chem.wisc.edu/research/nanofibers/index2.htmSarah BakerGrinnell ‘01UW ‘06
Teaching Analytical Chemistry at Grinnell
• CHM 130: Inorganic and Analytical Chemistry– Texts: Daniel Harris, Exploring Chemical
Analysis, 3rd Ed. and Luther Erickson, Water Module Guidebook
• CHM 358: Instrumental Analysis– Text: Skoog, Holler, Nieman, Principles of
Instrumental Analysis, 5th Ed.
Instrumental Analysis: Electrochemistry Labs
• Iodide Ion Selective Electrode
• Polarography of Pb
• Anodic Stripping Voltammetry
• Cyclic Voltammetry
• Rotating Ring Disk Voltammetry
• Impedance Spectroscopy
• Spectroelectrochemistry
CHM 130 Text Topics • Review of Monoprotic Acid/Base Equilibria• Titrations and Buffers• Polyprotic Acids• Activity• Spectrophotometry and Atomic Spectroscopy• Transition Metal and Coordination Chemistry• Chromatography and Mass Spectrometry• Nuclear Chemistry
Water Module Overview• 5 weeks of lab; 4 weeks of class• Question driven discussion of solubility
equilibria, carbonate equilibria, atomic spectroscopy, and electrochemistry
• Lab analyses of drinking water from around the country with Grinnell, Chicago, Des Moines, and bottled water providing benchmarks
• Lab concludes with student poster presentations
Water Module: Class Sessions (Week 1)
• Session 1. Formulating the Questions and Limiting the Exploration: Focus on Ionic Composition
• Session 2. Dissolved Ionic Solids: Which ionic salts are present in typical water samples and how did they get there?
• Session 3. Major species vs. minor species: Why are so many different concentration units employed to describe concentration levels of the several species present in water samples?
Water Module: Class Sessions (Week 2)
• Session 4. Carbon dioxide and dissolved carbonates: Why do virtually all fresh water samples contain bicarbonate as a principal species?
• Session 5. Hard water: What is meant by hard water and why does degree of hardness matter?
• Session 6. Sodium and yellow flames: How can we determine how much sodium is in the water?
Water Module: Class Sessions (Week 3)
• Session 7. Galvanic Cells and Ion Concentrations: How can galvanic cells be used to determine ion concentrations?
• Session 8. Potentiometric Titrations: How do ion concentrations change in the course of a titration?
• Session 9. Ion-Selective Electrodes and ppm Concentrations: How can we determine ion concentrations at the 1 ppm level?
Water Module: Class Sessions (Week 4)
• Session 10. Conservation of Mass and Charge: Does it all add up? (including poster preparation)
• Session 11. What does it all mean? What does the complete chemical analysis reveal about the source and treatment of our water samples?
• Session 12. Exam
Water Module: Laboratory• L1. pH and Alkalinity by Potentiometric Titration with
HCl• L2. Water Hardness (Total and Ca) by EDTA Titration• L3. Chloride by Potentiometric Titration with Silver
Nitrate• L4. Sodium Determination by Atomic Emission
Measurements• L5. Nitrate by Potentiometry with Ion Selective Electrode• L6. Fluoride by Potentiometry with Ion Selective
Electrode• L7. Total Dissolved Solids by Electrical Conductivity
Water Module Student Data
Location [F-] (ppm) [NO3-] (ppm) [Cl-] (ppm) [Na+] (ppm) [Ca2+] (ppm) [Hardness] (ppm) HCO3- (ppm) TDS (ppm) Calc. TDS
London 0.950 3.88 36.1 15.4 227 228 179 635 463 Chicago 6.08 0.238 14.6 2.92 83.1 123 104 318 251 Memphis 9.31 0.140 5.50 7.27 18.2 33.3 38.5 109 94 St. Paul 1.03 0.450 31.1 6.12 49 70.8 46.3 266 156 Chicago 6.65 0.448 15.6 2.35 81.2 186 99.1 315 310 Grinnell 10.8 0.448 28.4 255 42.2 96.7 240 1420 631 Des Moines 7.03 6.29 53.3 49.4 78.6 182 61.9 517 360
Dasani 0.190 0.196 4.27 0.0971 2.58 21.1 7.44 55.3 33.3
Gillis, Goodwin-Kucinsky, Patnaik, Peters, and Yohannes
Silicon Electrolytes for Lithium Battery Applications
Si Si
SiSi
OSiRC
Grinnell College
Lithium Battery Group
Argonne National Laboratory
Quallion, LLC
Sylmar, CA
In the News
• R&D 100 Award, September, 2005
• Scientists craft lithium batteries• by John Potratz• Badger Herald Wednesday, October 5, 2005
• New battery stimulates damaged nerves• By ASTARA MARCH• Science Daily, Oct. 3, 2005
Linear Polysiloxane Ionic Conductivities
Doping Level (Li / EO )
0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.14
log
σ
-5.25
-5.00
-4.75
-4.50
-4.25
-4.00
-3.75
-3.50
-3.25
-3.00
2 oxygens 3 oxygens 4 oxygens5 oxygens 6 oxygens 7 oxygens 8 oxygens
Si O
OO
OO
m
m
n
Macromolecules, 2001, 34, 931-934.
LiTFSI
Cross-linked Polysiloxane Gel Electrolytes
Si
CH3
H
O[ ] n
O OCH3
()3
Si
CH3
O[ ]m ( )OO 13+ CF S
O
O
N S
O
O
C F
F
F F
FLi +_
+
THF solution
LiTFSI
vacuum
12h
high Vacuum line
10-5 torr,48h
heating80oC,12h
SPETHF
10
30
50
70
90
1000150020002500300035004000
Wavenumber, cm -1-4.40
-4.20
-4.00
-3.80
-3.60
-3.40
-3.20
-3.00
4 14 24 34 44 54 64 EO / Li+
25 oC37 oC50 oC70 oC
Macromolecules, 2003, 36, 9176.
σ
Liquid Siloxane Electrolytes
- 1 1 5 . 0 0
- 1 0 5 . 0 0
- 9 5 . 0 0
- 8 5 . 0 0
- 7 5 . 0 0
0 . 0 0 0 . 0 2 0 . 0 4 0 . 0 6 0 . 0 8 0 . 1 0
L i : E O
T
g
(ºC)
4 . 3 a
3 . 3 a
3 . 4 a
4 . 2 a
O : L i = 3 2 : 1
O : L i = 1 0 : 1
u n d o p e d
O : L i = 3 2 : 1
O : L i = 1 0 : 1
O : L i = 3 2 : 1
O : L i = 1 0 : 1
u n d o p e d
Chem. Mater., 2006, 18, 1289.
Atlanta ACS Meeting
1000/T (1/K)
2.9 3.0 3.1 3.2 3.3 3.4 3.5 3.6 3.7
log (
σ)
-3.8
-3.6
-3.4
-3.2
-3.0
-2.8
-2.6
-2.4
1NM3 15:11NM4 10:11NM6 15:11NM7.2 10:1
VT Conductivities of 1NMx/LiTFSI
NMR Studies of Electrolytes
OO
OO
Si
h
h
g
ch
ef
ef d
ba
Li+/Eo
0.00 0.02 0.04 0.06 0.08 0.10 0.12 0.14 0.16 0.18 0.20 0.22
Δ δ ( ) ppm
-0.02
0.00
0.02
0.04
0.06
0.08
0.10
0.12
0.14
0.16
0.18
abcd & mef
abcd & mef
abcd & mef
abc
d & mef
1NM3
Acknowledgements: Grinnell College
Marie Mapes Douglas SchumacherFelipe Bautista Jay JinDavid Clipson Kate MorcomYanika Schneider Jacob BarreraLori Cooke Scott HarringMegan Straughan James TaggartT. Andrew MobleyNSF-REU, NSF-MRI (2), HHMI, Grinnell College3M
Luther E. Erickson, “The Water Module Guidebook”
Acknowledgements: Organosilicon Research Center
Robert West David Moline Richard HooperQinzheng WangDavid SherlockRyan West Zhengcheng ZhangNicholas A. A. RossiLingzhi Zhang
UW University-Industry Relations GrantNIST-ATP
Si Si
SiSi
OSiRC
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