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1、按一下以編輯母片標題樣式按一下以編輯母片副標題樣式 博博 精精 儀儀 器器熱分析技術熱分析技術 簡介簡介(DSC, TGA & DMA)(DSC, TGA & DMA)PerkinElmer Thermal Specialist 康瑜容 Tiffany KangTiffany.K博博 精精 儀儀 器器Thermal-Thermal-2 2 Differential Scanning Calorimetry (DSC) Thermogravimetric Analysis (TGA) Thermomechanical Analysis (TMA) Dynamic Mechanical Analy
2、sis (DMA)常用的熱分析方法博博 精精 儀儀 器器Thermal-Thermal-3 3常用的熱分析方法DSCHeatflowvs.Temp-Tm,Tc,Tg-H,curingtime,curingdegree-Reactionrate,kineticsTGAWeightLossvs.Temp-Decompositiontemperature-%Wtpercentage-OxidativetimeTMADimensionalChangevs.Temp-CTE(a1,a2)-Tg-SofteningpointDMAViscoelasticpropertyvs.Temp-Storage/Lo
3、ss/ComplexModulus(E,E”,E*)-tan-Viscosityandmastercurve博博 精精 儀儀 器器Thermal-Thermal-4 4博博 精精 儀儀 器器Thermal-Thermal-5 5高分子材料結構Type of Polymer Chain Structure (Continued)TypeStructureExampleTypeStructureExampleStarStarNetworkNetworkInterpenetratingInterpenetratingnetwork(IPN)network(IPN)Phenol-formaldehyd
4、eresinsPhenol-formaldehyderesinsTwocrosslinkedpolymersnotTwocrosslinkedpolymersnotbondedtoeachotherbondedtoeachotherCrosslinkedepoxywithvinylCrosslinkedepoxywithvinylpolymerpolymer博博 精精 儀儀 器器Thermal-Thermal-6 6高分子材料的分類PolystryenePolycarbonatePolyurethanesPolysulfoneAmorphousLOW/MEDIUMNylonPETAcetalH
5、IGHPPSPPHDPECrystallineThermoplastics(Nochemicalchangeonheating)EpoxiesPolyimidesPolyestersPhenolicsUncuredRubberSiliconesNeopreneEpoxyCuredThermosets(Chemicalchangeonheating)Polymers博博 精精 儀儀 器器Thermal-Thermal-7 7Amorphous vs. Crystalline?AmorphousAmorphousThermoplasticThermoplasticCrystallineCrysta
6、llinePolymerPolymer博博 精精 儀儀 器器Thermal-Thermal-8 8Semi-Crystalline PolymerSemi-CrystallineSemi-CrystallinePolymerPolymer Semi-crystalline polymers contain both amorphous AND crystalline phases Properties dominated by both Tg and Tm Semi-crystalline polymers can exhibit additional crystallization duri
7、ng heating博博 精精 儀儀 器器Thermal-Thermal-9 9Thermosetting Polymer博博 精精 儀儀 器器Thermal-Thermal-1010Schematic Results in Thermal AnalysisQualityofsampleprocessDSC(ExQualityofsampleprocessDSC(Ex) )TGATMADMATGATMADMA- -CrystallineCrystalline- -Semi-crystallineSemi-crystalline-Amorphous-Amorphous-Semi-crystall
8、ine-Semi-crystalline-General-General-Liquid-Liquid-Unspecific-Unspecific-SolidMelting-SolidMeltingRecrystallizationRecrystallizationSublimationSublimationSolid-solidtransitionSolid-solidtransitionGlasstransitionGlasstransitionSofteningwithoutTgSofteningwithoutTgPost-crosslinkingPost-crosslinkingDeco
9、mpositionDecompositionLigandreleaseLigandreleaseEvaporationEvaporationChemicalreactionsChemicalreactionsDeterminationof%Determinationof%按一下以編輯母片標題樣式按一下以編輯母片副標題樣式 博博 精精 儀儀 器器DSC TechniqueDSC TechniqueDifferential Scanning CalorimetryDifferential Scanning Calorimetry博博 精精 儀儀 器器Thermal-Thermal-1212Ques
10、tion? 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?博博 精精 儀儀 器器Thermal-Thermal-1313What 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
11、質。博博 精精 儀儀 器器Thermal-Thermal-1414Thermal Analysis applications - DSC- -Principle:Principle: Heat flow change vs. temperatureHeat flow change vs. temperature- -Measures:Measures: Phase transition ( Phase transition (TgTg, Tm, , Tm, TcTc) and heat ) and heat Curing reaction and other chemical reaction
12、s Curing reaction and other chemical reactionsDiamond DSCDiamond DSC博博 精精 儀儀 器器Thermal-Thermal-1515 Polymer TransitionsHeatFlowTemperatureTgStressReliefOrderingProcessCold CrystallizationCuringTmHDegradationStart upTransient博博 精精 儀儀 器器Thermal-Thermal-1616DSC Thermal Curve of PET吸 熱放 熱博博 精精 儀儀 器器Ther
13、mal-Thermal-1717DSC for curing studies Detection of Tg Onset of cure Maximum rate of cure (peak maximum) End of cure Heat of cure博博 精精 儀儀 器器Thermal-Thermal-1818DSC熱示差掃描分析儀之應用相變化點PhaseTransition熔融熱H玻璃轉移溫度Tg反應熱H熔點Meltingpoint活化能Ea冷結晶溫度CrystalTemperature氧化導引時間O.I.T.降溫結晶溫度ColdCrystalTemperature反應動力學Dyna
14、mic結晶度Crystallinity交連Curing結晶熱CrystalEnergy純度Purity結晶半週期CrystalPeriod比熱Cp博博 精精 儀儀 器器Thermal-Thermal-1919DSC的設計方式熱流式熱流式 Heat Flux DSCHeat Flux DSC熱補償式熱補償式 Power Compensation DSCPower Compensation DSC- -量測量測 T T- - 由由 H = H = k k T T計算計算 H H- - 爐體較大爐體較大- -直接量測直接量測 H H- - 不需複雜數學運算不需複雜數學運算- - 爐體較小爐體較小按一
15、下以編輯母片標題樣式按一下以編輯母片副標題樣式 博博 精精 儀儀 器器TGA TechniqueTGA TechniqueThermogravimetric AnalyzerThermogravimetric Analyzer博博 精精 儀儀 器器Thermal-Thermal-2121Thermal Analysis applications - TGAPyris 1 TGAPyris 1 TGA- -Principle:Principle: Weight change vs. temperatureWeight change vs. temperature- -Measures:Measu
16、res: Compositions and wt% Compositions and wt% Thermal stability and decomposition temp. Thermal stability and decomposition temp.博博 精精 儀儀 器器Thermal-Thermal-2222TGA Design Concept懸吊式懸吊式水平式水平式上置式上置式博博 精精 儀儀 器器Thermal-Thermal-2323TGA Thermal Curves博博 精精 儀儀 器器Thermal-Thermal-2424主要元件p Temperature control device - Furnace, Thermocouplep Weight measurement device -Null BalanceDetectorTare WeightSampleTorque MotorTGATGA 的設計原理的設計原理博博 精精 儀儀 器器Thermal-Thermal-2525TGA熱重分析儀 水份含量 溶劑含量 塑化劑含量 高分子添加物含量 裂解溫度 灰份
