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热分析技术分析


Ligand release
-Liquid -Unspecific Evaporation Chemical reactions Determination of % 博精儀器
Page 10
Thermal-10
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DSC Technique
Differential Scanning Calorimetry
-Semi-crystalline Sublimation Solid-solid transition -Amorphous Glass transition
-Semi-crystalline Softening without Tg
Post-crosslinking -General Decomposition
What is DSC ?
示差掃瞄熱卡量計 ( Differential Scanning Calorimeter ) : 將樣品置於特定氣氛之下改變其溫度環境或維持在一固定 溫度之中去觀察樣品其能量變化,當樣品發生熔融、蒸發、 結晶、相轉變等物理現象,或化學變化時,圖譜中將會出 現吸熱或放熱帶,進而可推測樣品之性質。
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Page 7
Thermal-7
Semi-Crystalline Polymer
Semi-crystalline polymers contain both amorphous AND crystalline phases Properties dominated by both Tg and Tm
Epoxies Polyimides Polyesters Phenolics
Rubber Silicones Neoprene Epoxy
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Page 6
Thermal-6
Amorphous vs. Crystalline?
Amorphous Thermoplastic
Crystalline Polymer
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熱分析技術 簡介
(DSC, TGA & DMA)
PerkinElmer Thermal Specialist 康瑜容 Tiffany Kang Tiffany.Kang@
常用的熱分析方法
Differential Scanning Calorimetry (DSC) Thermogravimetric Analysis (TGA) Thermomechanical Analysis (TMA) Dynamic Mechanical Analysis (DMA)
Type Linear
Structure
Example Poly(vinyl chloride), Polystyrene
Branched short chain
Polypropylene
Long chain branching
Polypropylene
Poly(imidazol pyrrolones) Ladder
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Page 2
Thermal-2
常用的熱分析方法
DSC Heat flow vs. Temp - Tm, Tc, Tg - DH, curing time, curing degree
- Reaction rate, kinetics
TGA Weight Loss vs. Temp - Decomposition temperature - %Wt percentage - Oxidative time TMA Dimensional Change vs. Temp - CTE (a1, a2) - Tg - Softening point
PARTIALLY CURED
TOTALLY CURED
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Page 9
Thermal-9
Schematic Results in Thermal Analysis
Quality of sample process -Solid -Crystalline Melting Recrystallization DSC(Ex) TGA TMA DMA
Semi-crystalline polymers can exhibit additional crystallization during heating
Semi-Crystalline Polymer
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Thermal-8
Thermosetting Polymer
UNCURED
Question? PE分成HDPE, LLDPE及LDPE - 結構有何不同? - 性質有何差異? - 結構和性質有何關聯性? 結晶的過程為何? 加工條件對結晶有何影響? 結晶度對透明度的影響? 添加劑的影響?
DSC可解決哪些問題?
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Page 12
Thermal-12
(Chemical change on heating)
Amorphous
Crystalline
Uncured
Cured
Polystryene Polycarbonate Polyurethanes Polysulfone
LOW/MEDIUM Nylon PET Acetal
HIGH PPS PP HDPE
DMA
Viscoelastic property vs. Temp
- Storage/Loss/Complex Modulus (E’, E”, E*) - tan d - Viscosity and master curve
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Page 3
Thermal-3
高分子材料結構
Type of Polymer Chain Structure
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Page 4
Thermal-4
高分子材料結構
Type of Polymer Chain Structure (Continued)
Type Star
Structure
Example Phenol-formaldehyde resins
Network Two crosslinked polymers not bonded to each other
Interpenetrating network (IPN)
Crosslinked epoxy with vinyl pal-5
高分子材料的分類
Polymers
Thermoplastics
(No chemical change on heating)
Thermosets
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