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Electrochromic Prussian Blue Thin Films (https://education.mrsec.wisc.edu/electrochromic-prussian-

blue-thin-films/)

Electrochromic Prussian Blue Thin

Films
Modified by Jason Marmon and
George Lisensky from J. J. Garcia-
Jareño, D. Benito, J. Navarro-
Laboulais, and F. Vicente,
“Electrochemical Behavior of
Electrodeposited Prussian Blue Films
on ITO Electrodes,”
(http://jchemed.chem.wisc.edu/Jour
nal/Issues/1998/Jul/abs881.html) J.
Chem. Educ., 75, 881-884 (1998).
Prussian Blue has been made by chemists for 300 Nanotechnology
hundred years. For more information on its history, Pages
see
http://webexhibits.org/pigments/indiv/overview/prussblue.html
(http://webexhibits.org/pigments/indiv/overview/p
russblue.html). In this experiment, K4[Fe(II)(CN)6]
Background
reacts with Fe(III)Cl3 in solution to give insoluble
Prussian Blue on the electrode. The approximately Nanotechnology
Application:
100 nm thick layer exhibits visible electrochromism, Space
and the coating on the glass changes color with Elevator
(https
applied voltage.
://edu
cation
Safety .mrse
c.wisc
Wear eye protection .edu/
nanot
echno
Procedure logy-
Step 1. (http://www.youtube.com/watch? applic
ation-
v=7v_qTwN9Ono#t=41) Add 5 mL 0.05 M HCl, space
then 10 mL 0.05 M K3[Fe(CN)6], and then 10 mL -
elevat
0.05 M FeCl3.6H2O to a 50 mL beaker. The mixed or/)
solution should be prepared just before use.
Nature:
The
Step 2. (http://www.youtube.com/watch? First
v=7v_qTwN9Ono#t=56) Identify the conducting Nanotechnologist
(https
side of a tin oxide-coated piece of glass by using a ://edu
multimeter to measure resistance. The conducting cation
side will have a resistance of 20-30 ohms. .mrse
c.wisc
.edu/
Step 3. (http://www.youtube.com/watch? natur
v=7v_qTwN9Ono#t=67) Face the conducting side e-
the-
of the glass towards a platinum wire coil or graphite first-
electrode. Connect the negative lead of a voltage nanot
echno
source to the glass and the positive lead to a logist
/)
 platinum wire coil or graphite electrode. Dip the Next
Big
electrodes (but not the aligator clips) into the
Thing
solution prepared above and quickly adjust the – All
voltage to produce 40µA/cm2 for 60 seconds. See About
Nano
electrical circuit diagram on another page. (https
://edu
Step 4. (http://www.youtube.com/watch? cation
.mrse
v=7v_qTwN9Ono#t=73) Rinse the electrode with c.wisc
pure water. The approximately 50 nm coating (see .edu/
next-
calculation) after 60 seconds of deposition can be
big-
seen by eye on the conducting surface. thing-
(The sixth term in the equation above comes from all-
about
the cubic unit cell dimensions. Inorg. Chem., 16(11), -
2704-2710, (1977)). nano/
)
Step 5. (http://www.youtube.com/watch? Smell:
v=7v_qTwN9Ono#t=87) Longer electrolysis times Sensing
on
give thicker coatings. In this movie, after passing the
80 µA current for 30 seconds (40µA/cm2 times an Nanoscale
(https
electrode area of 2 cm2) the electrode is rinsed to
://edu
show the color change. The rinsing steps are cation
repeated after every 30 seconds to show the .mrse
c.wisc
changing color but would not be needed otherwise .edu/s
unless you are recording visible absorbance (690 mell-
sensi
nm) as a function of layer thickness. The total
ng-
electrolysis time for this relative thick coating is on-
300 seconds. the-
nanos
cale/)
What area electrode did you use?
What
How much current for how long? is
Nanotechnology?
How thick is the film you produced? (https
://edu
cation
.mrse
:
 Step 6. (http://www.youtube.com/watch? c.wisc
.edu/
v=7v_qTwN9Ono#t=214) Place the rinsed
what-
electrodes in 25 mL 1.0 M KCl, keeping the clip is-
above the solution. Changing the applied voltage nanot
echno
changes the color of the thin film. logy-
defini
Step 7. (http://www.youtube.com/watch? ng-
nanot
v=7v_qTwN9Ono#t=220) Remove the battery echno
from the circuit and alternately connect the logy/)
electrodes as follows: Nanotechnology
Applications
1. Glass electrode connected to battery (–) and Video
(https
platinum or graphite electrode connected to ://edu
battery (+); negative voltage applied. cation
.mrse
2. Glass electrode directly connected to platinum c.wisc
.edu/
or graphite electrode; zero volts applied. Films
nanot
are reported to be more stable if you repeat echno
steps 1 and 2 several times before going on. logy-
applic
3. Glass electrode connected to battery (+) and ations
-
platinum or graphite electrode connected to video
battery (–); positive voltage applied. /)

4. Glass electrode directly connected to platinum Nanotechnology

Application:
or graphite electrode; zero volts applied. Space
Elevator
5. Repeat. (https
://edu
Step 8. (http://www.youtube.com/watch? cation
.mrse
v=7v_qTwN9Ono#t=275) Record the cylic c.wisc
voltammogram of the coated glass at 20 mV/sec .edu/
nanot
from +550 mV to -250 mV to +1200 mV to +550 echno
mV versus a Ag/AgCl reference electrode. When logy-
applic
ation-
space
:
 the voltage matches a redox reaction the current -
elevat
increases. Show cell and cyclic voltammogram
or/)
movies at the same time.
Nanotechnology
&
What color is the reduction product? What is Society:
the redox potential for the reaction? Ideas
for
Fe(III)4[Fe(II)(CN)6]3 + 4 K+ + 4 e- =
Education
K4Fe(II)4[Fe(II)(CN)6]3 and
Public
What color is the oxidation product? What is Engagement
the redox potential for the reaction? (https
://edu
Fe(III)4[Fe(II)(CN)6]3 + 3 Cl- = Fe(III)4[Fe(III) cation
(CN)6]3Cl3 + 3 e- .mrse
c.wisc
What is the source of the K+ and Cl- ions in the .edu/
nanot
redox reactions?
echno
logy-
Materials societ
y-
0.05 M HCl (Each preparation needs 5 mL. ideas-
Dilute 5 mL conc HCl to 250 mL with water.) for-
educa
0.05 M K3[Fe(CN)6] (Each preparation needs tion-
and-
10 mL. Dissolve 1.65 g in 100 mL water.) public
-
0.05 M FeCl3.6H2O (Each preparation needs engag
10 mL. Dissolve 1.35 g in 100 mL water with a emen
t/)
drop of HCl.)
Smart
1.0 M KCl (Each preparation needs 25 mL. Medicine
Dissolve 18.6 g in 250 mL water with two drops (https
://edu
of HCl to lower the pH.) cation
.mrse
Equipment c.wisc
.edu/s
50 mL beaker mart-
medic
Conductive Glass (1″ x 1″ x 2.3mm TEC 15 glass) ine/)
Hartford Glass Co, 735 E Water Street,
:
 Hartford City, IN 47348 Phone: 765-348-1282.
Glass can be reused by removing prussian blue
coatings with concentrated ammonia (solubility
increases with pH). Activities
Ohmeter Wheel
of
Pt wire or graphite electrode Fortune
Activity
1.5 Volt battery, holder, and 50 K ohm variable (https
resistor for controlling deposition current. See ://edu
cation
electrical diagram. .mrse
(http://education.mrsec.wisc.edu/Edetc/nanola c.wisc
.edu/
b/prussianblue/circuit.html)
wheel
-of-
Electrochemical apparatus for obtaining cyclic
fortu
voltammograms ne-
activi
ty/)
YouTube Link:
NanoSolutions
http://www.youtube.com/watch?v=7v_qTwN9Ono
Activity
(http://www.youtube.com/watch? (https
v=7v_qTwN9Ono) ://edu
cation
.mrse
c.wisc
.edu/
nanos
olutio
ns-
activi
ty/)
Applications
Activity:
Nanomedicine
(https
://edu
cation
.mrse
c.wisc
.edu/
applic
:
 ations
-
activi
ty-
nano
medic
ine/)

Applications
Activity:
“Smart”
Paper
(https
://edu
cation
.mrse
c.wisc
.edu/
applic
ations
-
activi
ty-
smart
-
paper
/)

Applications
Activity:
Nanocommunity
(https
://edu
cation
.mrse
c.wisc
.edu/
applic
ations
-
activi
ty-
nanoc
omm
unity/
)

Applications
:
 Activity:
Rocks
and
Nanobots
(https
://edu
cation
.mrse
c.wisc
.edu/
applic
ations
-
activi
ty-
rocks
-and-
nanob
ots/)

Applications
Activity:
Technology
and
Public
Policy
(https
://edu
cation
.mrse
c.wisc
.edu/
applic
ations
-
activi
ty-
techn
ology
-and-
public
-
policy
/)
:
 Video
Lab
Manual

Synthesis
of
Nickel
Nanowires:
Beaker
(https
://edu
cation
.mrse
c.wisc
.edu/s
ynthe
sis-
of-
nickel
-
nano
wires-
beake
r/)

Synthesis
of
Nickel
Nanowires:
Syringe
(https
://edu
cation
.mrse
c.wisc
.edu/s
ynthe
sis-
of-
nickel
-
nano
wires-
syring
e/)
:
 Titanium
Dioxide
Raspberry
Solar
Cell
(https
://edu
cation
.mrse
c.wisc
.edu/t
itaniu
m-
dioxid
e-
raspb
erry-
solar-
cell/)
Preparation
of a
Fuel
Cell:
Nafion
(https
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cation
.mrse
c.wisc
.edu/
prepa
ration
-of-a-
fuel-
cell-
nafio
n/)
Electrochromic
Prussian
Blue
Thin
Films
(https
://edu
cation
:
 .mrse
c.wisc
.edu/
electr
ochro
mic-
prussi
an-
blue-
thin-
films/
)

Tungsten
Trioxide
Intercalation
(https
://edu
cation
.mrse
c.wisc
.edu/t
ungst
en-
trioxi
de-
interc
alatio
n/)
Synthesis
of
Nanocrystalline
Y2O3:
Eu
Phosphor
(https
://edu
cation
.mrse
c.wisc
.edu/s
ynthe
sis-
of-
nanoc
rystall
:
 ine-
y2o3-
eu-
phosp
hor/)

Preparation
of
Surface
Conductive
Glass
(https
://edu
cation
.mrse
c.wisc
.edu/
prepa
ration
-of-
surfac
e-
condu
ctive-
glass/
)

Synthesis
of
Inverse
Opal
Photonic
Crystals
(https
://edu
cation
.mrse
c.wisc
.edu/s
ynthe
sis-
of-
invers
e-
opal-
photo
nic-
:
 crysta
ls/)

Preparation
of
Zeolite
ZSM5
and
Catalysis
of
Xylene
Isomerization
(https
://edu
cation
.mrse
c.wisc
.edu/
prepa
ration
-of-
zeolit
e-
zsm5-
and-
cataly
sis-
of-
xylen
e-
isome
rizatio
n/)
:
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