Part I DSC Perkin Elmer SVC Engineer Sam

熱分析技術客戶訓練 Part I : DSC Perkin. Elmer SVC Engineer 蔡傳盛 Sam Tsai Sam. tsai@perkinelmer. com

常用的熱分析方法 Differential Scanning Calorimetry (DSC) Thermogravimetric Analysis (TGA) Thermomechanical Analysis (TMA) Dynamic Mechanical Analysis (DMA) DSC-3

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 TMA - %Wt percentage - Oxidative time Dimensional Change vs. Temp - CTE (a 1, a 2) - Tg - Softening point DMA Viscoelastic property vs. Temp - Storage/Loss/Complex Modulus (E’, E”, E*) - tan d - Viscosity and master curve DSC-4

DSC Technology 熱流式 … DSC 4000/6000 系列 DSC-7

DSC Technology 熱功率補償式… DSC 8000/8500 系列 DSC-8

DSC熱示差掃描分析儀之應用 相變化點 Phase Transition 熔融熱 H 玻璃轉移溫度 Tg 反應熱 H 熔點 Melting point 活化能 Ea 冷結晶溫度 Crystal Temperature 氧化導引時間 O. I. T. 降溫結晶溫度 Cold Crystal Temperature 反應動力學 Dynamic 結晶度 Crystallinity 交連 Curing 結晶熱 Crystal Energy 純度 Purity 結晶半週期 Crystal Period 比熱 Cp DSC-10

DSC Thermal Curve 吸 熱 放 熱 DSC-11

DSC Lab System Example: DSC with Intracooler cooling system DSC-14

Sample Preparation DSC Sample Pan Various type: for solid, powder, liquid, volatile… Materials: Aluminum, Copper, Gold Platinum, Alumina, Graphite Large volume stainless steel sample pan DSC-15

Sample Preparation DSC Sample Crimper High pressure capsule sealing kit Universal Crimper Standard Crimper DSC-16

樣品大小影響靈敏度與解析度 100 Heat Flow (m. W) 75 50 25 0 Indium 4. 998 mg 10. 001 mg 20. 072 mg Peak = 158. 93 Peak from: 155. 50 to: 160. 50 Onset = 156. 51 J/g = 28. 51 Peak = 158. 30 Peak from: 155. 50 to: 161. 40 Onset = 156. 56 J/g = 28. 49 Peak = 157. 74 Peak from: 155. 50 to: 162. 70 Onset = 156. 54 J/g = 28. 71 145. 00 150. 00 155. 00 Temperature 160. 00 165. 00 170. 00 ( C) DSC-19

DSC數據計算方式 -- Peak DSC-22

DSC數據計算方式 -- Peak DSC-23

Tg 計算方法的差異 -- Tg PET 半比熱 75. 71 o. C 反曲點 78. 40 o. C 半寬 77. 04 o. C Fictive Tg 66. 40 o. C DSC-24

Tg 計算方法的差異 -- Tg Epoxy環氧樹脂 第二次加熱曲線 應力釋放 Stress Release 半比熱 78. 90 o. C 反曲點 82. 70 o. C 半寬 78. 90 o. C Fictive Tg 77. 80 o. C DSC-26

Polymer Transitions Stress Relief Heat Flow Tg Tm Cold Crystallization H Degradation Start up Transient Curing Ordering Process Temperature DSC-27

結晶與交聯的放熱反應 當材料發生交聯或結晶時，材料內部的亂度降低，自由能也降低成為較 穩定狀態，因此，當交聯或結晶發生時會伴隨發生放熱反應。 Tm Stress Relief Tg Heat Flow Start up Transient Cold Crystallization Ordering Process H Degradation Curing Temperature DSC-28

Thank you for your attention. DSC-31

熱分析技術客戶訓練 Part II : TGA Perkin. Elmer SVC Engineer 蔡傳盛 Sam Tsai sam. tsai@perkinelmer. com

TGA Design Concept 懸吊式 水平式 上置式 DSC-34

TGA 的設計原理 主要元件 Temperature control device - Furnace, Thermocouple Weight measurement device -Null Balance Detector Torque Motor Sample Tare Weight DSC-35

TGA Thermal Curves DSC-36

Perkin. Elmer TGA Model TGA 4000 STA 6000 (DSC/TGA 二合一機型) Pyris 1 TGA 標準爐 Ambient~1000 ℃ 高溫爐 Ambient~1500 ℃ DSC-38

STA 6000 Design 上置式設計 Top loading balance 新型 Sa. Turn. A™ Sensor 設計 DSC-39

TGA Lab System TGA Analyzer 主機 Purge gas 氣體 N 2, O 2, Air, He … etc. 氣體切換系統 Gas Switch, Gas station 控制軟體部分 樣品盤 DSC-49

TGA Lab System Example: Pyris 1 TGA & Optional Autosampler、Gas switch system DSC-50

Sample Preparation TGA Sample Pan Platinum Ceramic DSC-51

Thank you for your attention!