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Structure, dynamics and association of thermosensitive core shell particles [Elektronische Ressource] / vorgelegt von Jérôme Crassous

151 pages
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Geo
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Thermosensitive
F
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P
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rticles
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on
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der
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-
rankreic
Dr.
Ba
rer.
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nat.ter)
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hes
v
Dissertation.
orliegende
h
Arb
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eit
durc
wurde
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der
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Univ
der
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t
Ba
ommission:
yreuth
20.07.2009
in
H.
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Matthias
Zeit
Aksel
v
F
on
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bis
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Jan
die
uar
Wissensc
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ollo
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tierender
Lehrstuhl
Dr.
f?r
M?ller
Ph
Prof.
ysik
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he
eitgutac
Chemie
Dr.
I
Prof.
un
er
ter

Betreuung
Grades
v
doktors
on

Herrn
genehmigten
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Dissertation
Dr.
h
Matthias
am:
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angefertigt.
h
V
Promotionsk
ollst?ndiger
06.05.2009
Ab

druc
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quium:
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v
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uss:
Biologie,
Dr.
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Ballau
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h
Geo
Prof.
wissensc
Nuri
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(Zw
der
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Univ
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Andreas
Ba
ery
yreuth
Dr.
zur
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des
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rend
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mes
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p
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ro
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duit
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lui
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ts,
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lever,
admirable.
l'id?e
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et
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vous
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With
and
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wing
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ideas
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of

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nish
strong
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thesis
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Prof.
and
the
w
P
ould
t.
lik
for
e
trolled
to
An
express
Millard
m
for
y
for
gratitude
AFM
to
and
all
oTEM
of

them.
hnical
It's
family
m
alw
y
gratefully
great
aluable
pleasure
to
to
as
thank
SEM
Prof.

Matthias

Ballau
vibrator,
for
of
giving
Gro?
the

opp
w
ortunit
are
y
ts
and
in
freedom
herein.
to
Dr.
do
the

particularly
h
um
in
elop
this
in
in
A
teresting
supp
eld
t
under
arious
his
Christophe
sup
ut
ervision.
the
His
Elisab

with
and
Karlheinz
supp
ailabilit
ort
but
w
gratitude
ere
and
a
simply
great
eliev
help
hrinner
to
kno
alw
in
a
tribution
ys
umerable
impro
TEM
v
TEM
e
ell
the
for
qualit
I
y
ert
of
and
m
for
y
ork
w
electric
ork.
in
Thanks
the
to
W
him
hhold,
I
Dr.
realize
for
what
this
it
Sc
is
and
to
K
b
kno
e
exp
and
p
b

eha
laser
v
presen
e
w
as
to
a
Bosco,

Keralakis
her.
discussions
I
I
thank
to
Prof.
the
Nuri
er
Aksel
e
and
together
Dr.
exp
Lutz
p
Heymann
,
for
Mih
the

fruitful
and

sp
ts
pro
and
from
discussions
m

and
m

y
Sergiu
w
dev
ork
programs
and
and
for
I
sharing
D?ngfelder
their
w
exp
lot
erience
kindness,
in

the
a
eld
and
of
ort.
the
the
rheology
m
.
m
I
b
thank
for
Prof.
orts,
Matthias
ha
F
ys
uc
in
hs
Sc
and
are
his
ac

wledged
w
their
ork
v
ers

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and
er
en
Henric
attempts
h
get
and
and
Da
o-
vid
images
Ha
w
jnal
as
for
G??ler
the
the
v

ery
thank
fruitful
Norb

Willen
oration
her
in
Dr.
the
R?gisser
eld
the
of
w
the
on

piezo
and
axial
the
and
dev
the
elopmen
sense
t
group
of
Dr.
the
olfgang

ec
mo
Theresia
del
and
biased
Ludwig
on
henmann
the
the
mo
of
de
instrumen

Florian
theory
h
.
aiger
It
prof.
w
erner
as
?hler
a
ac
great
wledged
pleasure
the
to
erimen
w
their
ork
erformed
with
their

tribution
h
the
outstanding

scien

tists.
ted
I
I
w
ould
ould
e
also
thank
lik
John
e
Dr.
to
tonis
thank
for
Miriam
fruitful
Sieb
and
en
orations.
b?ger
am
for
thankful
her
Pierre

for
hnical
n
supp
b
ort
of
and
w
for
dev
the
ed
measuremen
and
ts
his
she
ertise
p
the
erformed
olymer
during
hemistry
her
to
Diplomarb
driana
eit.
ut
I
the
am
t
also
ort
thankful
the
to
she
Dr.
en
Alexander
to
Wittemann
vide
and

Jo
v

of
hen
y
Ring

for
to
the
Ro
syn
hette
thesis
to
of
Mih
the
for
system
eloping
I
the
used
for
during
SAXS
m
Cry
y
analysis.
Phd.
thank
I
eth
also
for
w

an
ork
t
a
to
of
thank
and
Dr.
and
Alexander
Lauten
Wittemann
h
for
his
his
v

y
e

suggestions
supp
and
Last

not
oration
least;
in
express
the
y
eld
to
of
y
the
mem

ers
asso
friends

their
Dr.
supp
Markus
and
Drec
for
hsler,
ving
Prof.
a
Ishi
b
T
ed
almon
me.
and
Marc.
Contents
.
1
.
Intro
.

.
1
.
2
.
Cha
.

.
4
.
2.1
b

.
of
.
the
.
degree
.
of
.

3.2.4
on
.
the
.

.
and
.
sw
.
elling
.
b
.
eha
54
v-
.
ior
.
of
.
thermosensitiv
Shear
e
.

.

ds
latexes.
.
.
.
.
and
.
2.3.4
.
.
.
w
.
.
.
.
.
.
.

.
piezo
.
.
.
3.1.1
.
.
.
.
.
.
4
.
2.1.1
.
In
.
tro
instrumen

.
.
.
.
.
.
.
.
.
.
glass
.
.
.
.
.

.
.
.
65
.
.
.
linear
.
.
.
.
.
.
.
e
.
.
.
.
.
b
.
.
.
.
.
.
.
shear
.
.
.
.
.
2.3.6
.
.
.
.
.
.
.
.
.
of
4

2.1.2
.
Exp
.
erimen
.
tal
.
.
.
.
.
.
.
.
.
.
3.1.2
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3.1.4
.
.
.
.
.
Visco
.
.
.
.
.
.
.
3.1.6
.
.
.
.
.
.
.
.
.
disp
.
and
.
.
.
.
.
.
5
.
2.1.3
65

.

.
kground
.
.
.
.
tal
.
.
.
.
.
3.2.3
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
70
.
olume
.
.
.
.
.
.
.
.
.
visco
.
vior
.
.
.
.
.
.
.
.
.
.
9
2.3.5
2.1.4
es
Results
.
and
.
discussion
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
52
.
3.1
.
visco
.
vior
.
using
.
axial
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
tro
11
.
2.1.5
.
Summary
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
Instrumen
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
of
.
and
.
.
.
.
.
.
.
57
.
uids
.
.
.
.
21
.
2.2
.
Quan
.
titativ
.
e
.
analysis
.
of
.
p
.
olymer
.

.
b
.
y
.
normal
.
and
64

of
o-transmission
at
electron
in

o
y
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
In
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
Exp
.
and
.
.
.
.
.
.
.
.
.
.
.
and
.
.
.
.
.
.
.
.
.
.
.
.
.
.
22
.
2.2.1
.
In
.
tro
.

.
.
.
.
.
.
.
.
Eectiv
.
v
.
fraction
.

.
.
.
.
.
.
.
.
.
.
.
.
.
43
.
Linear
.

.
eha
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
48
.
Flo
.

22
and
2.2.2
melting
Exp
.
erimen
.
tal
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
51
.
Summary
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3
.
53
.
Characterization
.
the
.

23
eha
2.2.3
of
Theory
uids
.
the
.
electric
.
vibrator
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
53
.
In
.

.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
24
53
2.2.4
Theory
Results
.
and
.
Discussion
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3.1.3
.
ts
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
32
.
2.2.5
.
Summary
.
.
.
.
.
.
.
.
56
.
Calibration
.
the
.
t
.

.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3.1.5
.

.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
58
41
Summary
2.3
.
Crystallization
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3.2
.
stresses
.

.
ersions
.
the
.
transition
.
equilibrium
.
in
.
w
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
42
.
2.3.1
.
In
.
tro
.

.
.
.
.
.
.
3.2.1
.
tro
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
3.2.2
.
erimen
.
system
.
metho
.
.
.
.
.
.
.
.
.
.
.
.
.
.
42
.
2.3.2
.
Exp
66
erimen
Linear
tal
non
.
rheology
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
67
.
Theory
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
43
5
2.3.3.
Con
.
ten
.
ts
126
3.2.5
.
Comparison
.
of
.
theory
.
and
een
exp
.
erimen
.
t
.
.
.
.
.
.
.
.
.
.
ormation
.
.
.
.
.
.
.
.
.
Exp
.
.
.
.
.
.
.
4.2.4
.
.
.
.
.
9
82
.
3.2.6
.
Summary
.
.

.

.
gels
.
.
.
.
.
.
.
In
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
and
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
Synopsis
.
129
.
6
.
.
.
.
.
.
.
.
.
.
.
.
96
110
4
ole
Asso
y

et
97
osite
4.1
Gold
Rev
.
ersible
.
self-assem
.
bly
.
of
.

.
osite
112


.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
112
.
tal
.
.
.
.
.
.
.
.
.
.
.
.
97
.
4.1.1
4.2.3
In
.
tro
.

.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
121
.
6
.
Abb
.
Publications
.
rung
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
97
4.2
4.1.2
Dip
Coagulation
F

b
.
Asso
.
b
.
w
.
Comp
.

.
and
.
Nanoparticles
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
4.2.1
.
tro
.
.
.
.
.
.
.
.
98
.
4.1.3
.
Exp
.
erimen
.
tal
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
4.2.2
.
erimen
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
113
.
Results
.
Discussion
.
.
.
.
.
.
100
.
4.1.4
.
Results
.
and
.
Discussion
.
.
.
.
.
.
.
.
.
.
114
.
Summary
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
5
.
123
.
Zusammenfassung
101
7
4.1.5
reviations
Summary
8
.
143
.
Erkl?
.
145
.
.N
o
φeff

of
as

the
ed
if
p
e
oly(
inatable

ys
-isoprop
h
ylacrylamide)
the
(PNIP
ension
AM)
b


hains
o

sc
un-
the
dergo
us,
a
b
phase
of
transition
[42,
as
preparation
function
us
of
scales
temp

erature
ha
in

whic
trated
h
v
the
PNIP
net
w
w
leads
ork
shrinks
shrinks
h
in
in
a
rather

the
tin
[34].
uous
sphere
or
eha
discon
v
tin
Also,
uous
b
fashion.
again.
The
b
v
[34].
olume
the
transition
[31
in
thermosensitiv

renew
net
in
w
the
orks
ha
has

b
erall
een
these
studied
in
extensiv
particles
ely
is
b
the
y
ond
T.
olume
T
ork
anak
elling
a
v
and
olume
others
through
[1,
dense
2].
ed
A
y
review
et
on
t
w

ork
tages
done
er
on
previous
these
the

hand:
systems
situ
w

as
to
giv

en
simply
some
temp
time
the
ago
olume
b
and
y
equilibrium
Shiba
generated.
y
that
ama
e

the
Starting
other
with
32
early
,
w

ork
e
b
in
y
del
T
for
anak
study
a


b
man
of
y
ensions
groups
1.1
ha
o
v
and
e
transition
dev
in
elop
fashion:
ed
ater
syn
of
theses
sw
of
temp

w.
thermosensitiv
er,
e
erature
net
b
w

ork
a
b
in
y
net
e.g.
the
em
y
ulsion
ater.
p
eectiv
olymerization.
fraction
T

w
the
o
e
t
temp
yp
system.
es
ensions
of
ac
particles
of

state
b
w
e
erature.
prepared:
w
Either
to
the
v
par-
rheology



adv
totally
these
of
o
a

PNIP
used
AM-net
v
w

ork
w
[512
are

dense
or
generated
the
us
PNIP
shear
AM-net
deformation
w
lling
ork
rheometric
is
previous
p
y
olymerized
ension
on
e
to
raising
a
and
solid
w

olume
[1320
high


A
adjusted
great
pristine
n
in
um
all
b
b
er
et
of
w
p
"rev
ossible

applications
to
ha
for
v
asso
e
with
b
particles
een
,
discussed

for
tly
these
the
systems
e
that
particles

v
widely
attracted
separate
ed
elds
terest
as
mo
e.

g.
particular
protein
a
adsorption
e
[19,
of
20


and
They
w
ha
e-
v
vior
e

also
susp
b
[3341
een
Fig.

displa
tly
the
used
v
as

a
the
template
olume
for
of
the
particles

a
of

metal
Immersed
nanoparticles
w
[2123
the

AM-shell
for
the
applications
will
in
ell

the
[22,
erature

lo
A
Ho

ev
e
raising
review
temp
on
in
the
system
applications
ey
w
32
as
C
giv
to
en
v
b
transition
y
whic
Ly
the
on
w
[24
in

shell
They
b
presen
exp
t
w
a
Th
v
the
ersatile
e
Gels
olume
osed
Intro
1
ing
phase
determin-
b
the
eha
ydro
vior:
v
on
of
one
particles
hand
b
they
adjusted

the
b
erature
eha
the
v
Hence,
e
susp
lik

e
e
hard
hiev
sphere
out
with
a
a
dilute
liquid-crystal
b
transition
lo
b
ering
elo
temp
w
Sen
the
al.

ere
temp
rst
erature
presen
[7,
in
9,
estigations
25,
the
26
of

h
On
particles
the
The
other
an
hand
of
in
thermosensitiv
the
particles
absence
v
of
the

hard
stabilization
particles
or
in
in
in
saturated
estigations
salt
43

of
trations
o
the
b
particles
vior
b
at
ecome
The
attractiv
susp
e
is
after
in
the
th
lo
a
w
oiding

and
solution

temp
during
erature.
and
This
in
leads
a
to

a
all
partially
history
or
b
totally
shearing
rev
susp
ersible

aggregation
b
of
erased
the
y
system
the
in
erature
the
th
dilute
lo
regime
ering
and
v
to
fraction
the
The
gelation
v
of
fraction
the
then
system
e
for
again
higher
a

sample
trations
eing
[27
full
30].
at
The
length
ne

tuning
e
of
Sen
their
al
in
sho

ed
p
these
oten
ersibly
tial
spheres"

b
also
used
b
study
e
1
used
η γ˙
γ˙
η0
ηs
η/ηs
hapter
tr
b
ansition
e
in
hapter

.
or
and
e-shel
in
l
a

ed.
onetworks:

The
of
p
(cry
olymer
quan

y
ar
of
e
visco
axe
in
d
First
to
titativ
the
of
surfac
ork.
e
the
of
b
the
of

metho
or
oTEM
e.
observ
dep
y
endence
the
of
the
the
in
viscosit
brigh
y
the
volume
the
on
v
the
of
shear
er,
rate
theory
the
t
of

.
b
If
is
the
w
eectiv
thermosensitiv
e
transition
v
transmission
olume
endence
fraction
the
of
v
the
dev
particles
the
is
to
not

to
to
o
scattering
high,
part
a
the
rst
part
Newtonian
the
r
or
e
up
gion
to
is

observ
In
ed
an
if

the
o
shear
theory
rate
of
esentation
of
epr

is
put
small.

Here
fully
the

viscosit
,
y
exp
r
a

t
of
ha
the
een
susp
this
ension
w
measured
to
in
particles.
this
presen
rst
study
Newtonian

regime
v

Figure
b

e


The
tly
the
larger
and
than
erature
1.1:
rst
Figure
A
the
w
one
ed
of
ely
the
and
pure
in
solv
to
en

t.
dieren
A
are
t
obtained
higher
ligh
shear
small-angle
rates,
The
the
the
p

erturbation

of
The
the
the

system
of
y
the
transition.
susp
purp
ension

b
presen
y
rst
the
the
adv
y
ectiv
on
e
frequency
forces


this
no
terpretation
longer
of
b
disp
e
and
restored
biased
b
de
y
dev
the
last
Bro
thesis
wnian
the
motion
asso
of
temp
the
self-asso
particles.
system
Hence,
scrutin

the
t
2
she
no
ar
quan
thinning
e
will
of
result
[44
in
45
whic
and
h
erimen
the


discussion
viscosit
the
y
parameters

not
tro
v
In
b
1
done
study
efore
this
w
osite
This
The
ork
part

es
the

of
is

more
particles.
and
rst
more
describ
lo
the
w

ered
the
un
Here
til
e
one
t
ma
rst
y
of
sp
e
eculate
particles
that
their
a
olume
se
(cf.

1.1)
ond
y
Newtonian
ogenic
r
electron
e
y
gion
o-TEM).
is
dep
reac
on
hed.
degree


tly
on
,
temp
Sen
has
's
een
data
in
[34
estigated.

new
ha
d
v
as
e
elop
b
to
een
titativ
used
analyzed
to
TEM

Cry

images
k
order
the

predictions
the
of
ternal
mo
of
de-coupling
The
theory
t
(MCT)
ation
[44,

45
data

b
for

the
t
o
and
w
X-ra
b
scattering.
eha
last
vior
of
of


fo
trated
on
susp

ensions
of
[39
particles.
,


explores
Go

o
this
d
in
agreemen

t
of
w
glass
as
F
reac
this
hed
ose
in
new
this
set

is
emplo
ted
ying
the
sc


measure
MCT
linear
mo

dels
of
[39].
uids
Hence,
a
this
t

range.
suggests
the
that

the
of
thermosensitiv
part,
e
in
particles
of
sho

wn
the
in

Fig.
ersion
1.1
equilibrium
presen
in
t
w
an
on

mo
t

mo
is
del
elop
system
The
for
part
the
the
study
in
of
estigates
the
eld

the
of

susp
the
ensions
erature
in
trolled
the


the
y
is
of
under
the
y
glass
Then
transition.
asso
Ho
of
w
evb
these
nanoparticles

discussed.
osite
will

e
with
3
gold′N N,N
o

the
m
degree
e
of
system

large
on
,
the
v

de-coupling
and

sw
ts
elling
in
b
[17
ehavio
to
r
y
of
[39,
thermosensitive
further

oin
re-shell
y

tal
latexes.
as
2.1.1
34
Intro
resonance

,
En
gels,
vironmen
ev
tally

sensitiv
us
e
v

b
ha
vide
v
systems
e
the
attracted
of

elucidation
in
e
terest
sub
due
er
to
t
their
prop
abil-
55
it
[5557
y
erimen
to
as
sw
t
ell
,
and
y
de-sw
64].
ell
understanding
in
adv
resp
hapter
onse
study
to
solution.
external
syn
stim
65
uli
59

used
h
of
as

temp
obtained
erature,
test
pH

or
44,
ligh

t
particles.
radiation
of
[4648
w

in
A
e
great
this
n
ogenic
um
een
b
of
er
um
of
exp
p
in
ossible
ears.
applications
the
ha

v
y
e
high
b

een
rheology
discussed
to
for
probing
these

systems.
uclear
A


[7,
e
,
review
56,
on
small-angle
the
neutron
applications
49,
w
to
as
degree
giv

en
h
b
ho
y
This
Na
dev
y

ak
thermosensitiv
and
in
Ly
particles
on
b
[24].
b

,
of
and
p
[13
oly(
They
of
b
-isoprop
mo
ylacrylamide)
the
(PNIP
o
AM)
vior

susp
ed
The
b
far
y


the
2.1
of

dense
Cha
40
-

meth
oin
ylenebisacrylamide
tion
(BIS)
of
ha
en
v
the
e
particles
b

een
this
of
is
particular
of
in
will
terest.
in
The
2.3.
temp
hapter
erature
that
of
electron
the
o-
v
the
olume

transition
a
is
n
lo
b

of
at
erimen
32
studies
2

in
y
estigations
The
from
v
C
range
in
measuremen
aqueous
of
solution

whic
erties,
h
h
mak
turbidit
es
[54,
them

suitable
sensitiv

scanning
didates

for

p
[7,
ossible


exp
applications
ts


h

as
h

n
trolled
magnetic
release
[56,
systems
ligh
[19,
scattering

13
Other
34
applications
49

55,
e.g.
58
the

use
X-ra
of
and

scattering
h
,
systems
59
as
Compared


for
the
metallic
of
nanoparticles
of
in
is

uc
[22,
less


The
w
v
er.
olume

transition
is
in
oted

a
net
e
w
of
orks
e
has
particles
b
aqueous
een
These
studied
ha
extensiv
e
ely
een
b
thesized
y
y
T.
[17
T
63
anak

a
b
and
others
others
,


A
ha
thermo
e

een
analysis
as
of
del
the
for
transition
study

the
b
w
e
eha
done
of
in
trated
terms
ensions
of

the
results

so
Flory-Rehner
pro
theory
an
[49
t
53].
for
Hence,
mo
the
theory
v
the
olume
of
transtition

in
[39,

,
gels
45
seems
A
to
p
b
t
e
atten
rather
is
w

ell
these
understo
Giv
o
the
d.
that
F
shell
or
these
details

the
a
reader
net
is
ork,
deferred
p
to
t
the

review
need
of
further
Shiba
and
y
b
ama
discussed

the

hapter
with
In
dimensions

in
w
the
demonstrate


domain
transmission
ha

v
(Cry
e
4
b

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