1. DTA, Differential Thermal Analysis

1 1/13 Kumnong Engineering Electronical measuring instruments Mechanical measuring instruments Hadaewondong. 139-3 2F Jungwonku. SeongnamCity. KyungkiDo. 462-839. Korea. 2 Tel #82-31-756-7320 Fax #82-31-758-4998 1. DTA, Differential Thermal Analysis ( Differential Thermal Analysis ; DTA) (furnace) (temperature difference) (thermocouple) ( 1).. 1. DTA heating block. S: sample, R: reference heating block ( : ).. 2/13 ( ) ( 2_ ) . 2: DTA Tr (plot) DTA curve ( 2_ ). (exothermic reaction).

2 DTA curve 3 DSC (peak) step . , 3/13 DSC mW (heat flow) , DTA DTA DSC . SDTA (single DTA) .. SDTA TGA TMA, DMA . TGA TMA, DMA curve . TGA SDTA / . TGA . 3: DTA curve: 1 initial displacement, 2 melting, 3 exothermic chemical reaction 2. 2. 2. 2. (DSC, Differential Scanning Calorimetry)(DSC, Differential Scanning Calorimetry)(DSC, Differential Scanning Calorimetry)(DSC, Differential Scanning Calorimetry) (DSC) (inert reference) (difference in heat flow).

3 Heat Flux DSC (furnace)4/13 pan ( Thermal loss) pan . (Heat flow) (transmitted power) (W; Watt) (mW) . mW s mJ . (enthalpy) . , endothermic exothermic . DSC (enthalpy changes) ( Thermal effects) DSC , (fusion melting)- ( H), melting point(Tm), (glass transition temperature, Tg), (crystallization)- , (degree of cryatallization), (Tc), (curing)- (degree of cure), , postcuring, evaporation, solid-solid transition, polymorphism, oxidation-Oxidation Induction Time(OIT, ), Thermal stability, purity( ), identification, , (chemical reaction) , (specific heat).

4 DSC , (glass transition temperature, Tg) (heat capacity) baseline shift . DSC . DSC ( pan) / (dynamic) 5/13 (isothermal) . (temperature segment) . DSC curve: 1. initial startup deflection, 2. glass transition, 3. crystallization, 4. melting, 5. vaporization, 6. decomposition curve deflection(1) . stand-by (isothermal) (transient) startup deflection . Startup deflection . Startup deflection (heat capacity).

5 (heat capacity) endothermic step(baseline shift)(2) . (3) exothermic peak . endothermic peak . (chemical reaction) exothermic endothermic peak . endothermic peak(5) .. peak 6/13 pan . Open pan pan(hermetica lly sealed pan) . (decomposition) . purge gas type .. (inert; N2, Ar, He) (air, O2) . gas . (transition) (reaction) - . (curing).

6 Thermoplastic ( Thermal history) (enthalpy relaxation) peak . (edible fat) DSC curve: 1. initial deflection, 2. no Thermal effects, 3. melting peak, 4. oxidation onset 7/13 3. Thermomechanical Analysis3. Thermomechanical Analysis3. Thermomechanical Analysis3. Thermomechanical Analysis (TMA, (TMA, (TMA, (TMA, )))) TMA TMA TMA TMA TMA(Thermomechanical Analyzer, ) (dimension changes) . Dilatometry (load) stress TMA zero Newton (expansion) (shrinkage) . (LVDT; Linear Variable Differential Transformer) , (glass transition).

7 8/13 TMA (deformation) , (constant load) Dynamic Load TMA(DLTMA) (Young's Modulus) . DLTMA (viscoelastisity) . TMA dilatometric ( , CTE; Coefficient of Linear Thermal Expansion), (glass transition), , (volumetric changes) (polymophic deformation) . TMA TMA TMA TMA Thermal Expansion Glass transition, softening Phase transitions(solid-liquid, solid-solid) Melting point Polymorphism Thermal stability Young's modulus(dynamic load ) TMA DiagramsTMA DiagramsTMA DiagramsTMA Diagrams 1. TMA curve(under low comprehensive stress): 1. , 2.

8 ( ), 3. , 4. plastic deformation 9/13 2. Packaging film( ) TMA curve: 1. , 2. (plastic deformation) 3. PVC(polyvynyl chloride) TMA curve: PVC softening 10/13 4. Thermogravimetric Analysis4. Thermogravimetric Analysis4. Thermogravimetric Analysis4. Thermogravimetric Analysis (TGA, (TGA, (TGA, (TGA, )))) TGA(Thermogravimetric analyzer)TGA(Thermogravimetric analyzer)TGA(Thermogravimetric analyzer)TGA(Thermogravimetric analyzer) (TGA) (changes in mass) . (vaporization) (chemical reaction) . TGA purge gas (N2, He, Ar) (O2, air) (oxidation decomposition) purge.

9 (electronic balance) .. TGA (horizontal) (vertical) . TGA buoayncy drag force blank curve subtraction . Buoyance effect . 1. Horizontal TGA diagram 11/13 2. Vertical TGA diagram TGA (inert atmosphere) (combustion profile) . Coupling technique EGA(Evolved Gas Analysis ) . , TGA Mass Spectrometer(MS) Fourier Transform Infrared Spectrometer(FTIR) coupling . TGA DTA weight change (endothermic) (exothermic) . ( , ), , (carbon black), carbon fiber, (ash), filler( ) (compositional Analysis ) , (decomposition kinetics).

10 12/13 3. TGA curve: 1. , 2. pyrolysis, 3. ( ), 4. (residue) weight loss step (% ug, mg) . (residual solvent), . (gas pressure) . ( ) . TGA curve weight loss step DTG(Derivative TG) curve peak DTG curve slope . gas . (reactive condition) (gas exchange) . 13/13 4. TGA curve: 1. , 2. , 3. , 4. 5. TGA curve: 1. , 2. ( ), 3. carbon black , 4. : NAVER : NAVER : NAVER : NAVER iNiNiNiN