4.4 열분석contents.kocw.net/KOCW/document/2015/pusan/kimho… · · 2016-09-094.4 열분석...
Transcript of 4.4 열분석contents.kocw.net/KOCW/document/2015/pusan/kimho… · · 2016-09-094.4 열분석...
-
4.4
(Thermal analysis)
.
, DDTTAA ((DDiiffffeerreennttiiaall TThheerrmmaall
AAnnaallyyzzeerr)),, DDSSCC ((DDiiffffeerreennttiiaall SSccaannnniinngg CCaalloorriimmeettrryy)),,
TTGGAA ((TThheerrmmooggrraavviimmeettrriicc AAnnaallyyzzeerr)),, TTMMAA ((TThheerrmmoo
mmeecchhaanniiccaall AAnnaallyyzzeerr)) ,
DDMMAA ((DDyynnaammiicc MMeecchhaanniiccaall AAnnaallyyzzeerr)),,
DDEEAA ((DDiieelleeccttrriicc AAnnaallyyzzeerr)) .
DTA DSC
DTA
(Sample) (Reference)
(T) , DSC 0
(dQ/dt) , (T) (t) . ,
TT ((DDTTAA)) oorr ddQQ//ddtt ((DDSSCC)) vvss TT
-
DTA ,
, DSC
.
DSC Cell
,
0.5 ~ 10 mg (pan)
cell .
,
.
-
DTA 0
. , .
Enthalpy.
,
(Glass temperature: Tg), (Crystallization
temp.: Tc), (Melting temp.: Tm)
-
.
Tc Tm
, Tg
.
(a)
,
(b)
.
-
Tm enthalpy (H) .
.
HHaa -- HH XXcc == ------------------------ ,, HHaa:: eenntthhaallppyy HHaa -- HHcc HHcc:: eenntthhaallppyy
enthalpy Polymer handbook
, 2
.
>
2
x=0 x=1
y
.
-
TGA TMA
TGA (Thermogravimetric Analyzer)
, , ,
.
TMA (Thermal Mechanical Analyzer)
,
,
.
-
DMA (Dynamic Mechanical Analyzer; Rheovibron)
.
, .
() (: ) , .
Sensor
Stress analysis110 Hz
Sinusoidal strain
-
.
(Modulus: E)
(Stoage modulus; E) (Loss modulus: E)
,
EE == EE ++ i EE i o () () () .
o
o
-
,
== oo ssiinn wwtt,, == oo ssiinn wwtt
, == oo ccooss dd,, == oo ssiinn dd
EE == oo // oo
EE == // oo == EE ccooss ,, EE == // oo == EE ssiinn
,
EE ttaann == --------
EE
.
-
, E, E, tan , , . X-
DMA .
Distribution
of segment
Intramolecular
factor
Crystalline effect
Increasing resistance
of mobility
(chain length)
Increasing mobility of
relaxing segment
(number)
Intermolecular factor
-
Tan (transition), (Chain segment movements) . (Tg)
,
. ( )
(Segment length)
. (Shoulder curve)
.
E ,
E .
Styrene-Butadiene-
Styrene block polymer (SBS elastomer)
, , . ,
,
.
ccaassttiinngg ssoollvveenntt:: :: mmeetthhyyll eetthhyyll kkeettoonnee
:: eetthhyyll aacceettaattee
:: ttoolluueennee
:: ccaarrbboonn tteettrraacchhlloorriiddee
-
DEA (Dielectric Analyzer)
,
, . , ,
(Cap (Conductance) ,
(
acitance)
.
.
:: ,, :: )
-
(I) (phase angle shieft; ) . (IIaa) (IIoo) .
((CCaappaacciittaannccee,, ffaarraaddss)) :: CC == (( IIaa // VV )) (( ssiinn // 22 ff )),, [[ ff :: HHzz ]] ((ccoonndduuccttaannccee,, oohhmmss)) :: 11 // RR == (( IIoo // VV )) ccooss
dipole () , dipole () . ,
, IIoo // IIaa == // == ttaann
, ,
.
-
Polymethylmethacrylate (PMMA) DEA .
, 100Hz~100kHz , . 17.7 kcal/mol .
-
4.5
, , X- ,
.
, ,
,
( ) .
(Density Gradient Column)
.
(A B)
.
,
,
.
-
, (Glass bead) ,
, . ,
, .
,
.
,
.
.
(cc) (aa) , .
cc ggllaassss bbeeaadd
XX == -------------- cc aa
ssaammppllee
.
-
GPC (Gel Permeation Chromatography)
Polystyrene Gel (Columns)
, ,
. Mn, Mw
.
.
gel (pore size)
column
, gel
, ,
.
, (, ) (, )
.
0.1 ~ 0.5%, 1
2 ml .
p115
-
GPC ,
GPC
.
-
UTM (Universal Testing Machine)
, ( ,
, ) , ,
.
Jaw
Cross-bar ,
Load cell
Data system
.
, , , ,
, , , , ,
.
-
(Stress-Strain curves) .
Controller
Sample
Clip, jaw
Load cell
Cross-head
-
- ,
, ,
,
(Modulus),
(Work; ) .
Data
-
Atomic Absorption Spectrophotometer (AA)
() ,
. Cu, Ge, Fe, Na, Pb, As, Al, Ni, Cr, Cd, Mn, Mg Na
.
, .
,
.
.
AA .