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 .