Thermal Analysis (TA) has become an indispensable family of analytical techniques in the polymer research. The increased importance of these techniques can be seen as the result of three more or less parallel developments:
• a tempestuous development of TA measuring techniques in combination with a high degree of automation,
• the strongly increased understanding of the underlaying theory and,
• the increasing knowledge of the relation between the polymers' chemical structure and their physical properties.
These areas are still in their developmental stages, especially the third area. The increasing knowledge of the dependence of physical properties on chemical structure just accentuated more and more the need for accurate thermoanalytical measurements, and this knowledge is very important for the first stages of the development of new polymeric systems. Besides, the contribution of TA remains necessary for the technical and commercial development of such a new polymer system. The use of the various TA techniques in these processes is described in this book in nine chapters, while chapter ten illustrates the information obtained about different polymers during special case studies.
This book illustrates in this way, applications of a wide variety of TA techniques whilst it is written from a materials characterisation rather than from a TA point of view with attention being paid to the chemical structure/physical properties correlations.
For those who work in the thermal analysis area in the context of polymer research.
Characterisation of Polymers by Thermal Analysis, 1st Edition
Preface. Acknowledgements. Chapter 1. Differential Scanning Calorimetry
. DSC calibration and stability. The Tg-value determination. Melting and recrystallisation determinations. The Tg-value of BR and SSBR rubbers. The Tg-value of BR and SSBR rubbers after blending and oil-extension. Additives acting as nucleating agents for PP. Annealing experiments with i-PP. Crystallisation in poly(1-olefine)s. The determination of the cure conditions of a powder coating system. Reactions of model compounds studied by DSC. DSC modification for the delta-Hvap.25 determination. Results of delta-Hvap.25 determinations by DSC. Chapter 2. Thermogravimetrical Analysis
. The non-isothermal thermal stability determination. The isothermal thermal stability determination. A 'plastic wrapped' TGA. TG analysis of a MgCl2-supported, TiCl4/DIBP catalyst. Chapter 3. Thermodilatometry
. The l.e.c. determination of filled polymers. Shrinkage of a PK terpolymer and Nylon 6.6 due to moisture loss. The volume dilatometer. The volume dilatometer measuring procedure. Isothermal crystallisation of IR rubbers. Chapter 4. Dynamic Mechanical Analysis
. DMA analysis of PP/C2C3 rubber blends. Tg-value determination of aged, rigid PU foams by DMA. Ultra-sonic measurement equipment. Results of ultra-sonic measurements on car-tyre rubbers. Chapter 5. Thermo-electrometry
. Dc properties of polymers. Ac properties of polymers. The ac and dc measuring system. Ac and dc properties of a cured resin system. Time/temperature superposition of dielectric results. The dielectric constant of rigid PU foam. Influence of moisture on the dielectric properties of resin castings and laminates. Effect of seawater and cargo on the electrical properties of a tankcoating system. The determination of the Ki-value of a PVC cable insulation. Electrostatic safety criteria. Dc properties of experimental epoxy resin/carbon black systems. Dc properties of anti-static epoxy GFR pipes. The TSD technique. Bucci's TSD theory. Results of TSD experiments. Chapter 6. Coupled Thermal Analysis Techniques
. The TSD/TMA system. TSD/TMA results. The TGA/FTIR and TGA/MS coupling. The heated capillaries tip temperatures. Single component calibration. Investigation of decomposition of cobaltphthalocyanine by TGA - coupled - FTIR/MS. Investigation of the released vapours during the cure of an epoxy resin system by TGA - coupled - FTIR/MS. Chapter 7. Chemical Structure/Physical Properties Correlations
. Introduction. The 'modified cohesion energy' Tg-value calculation method. The Tg-value of crosslinked polymeric systems. Reduced Tg/Tm correlations. The Hf-value estimation. The semi-static Td,o-value determination. Thermal stability estimation based on Td,o-values. The moisture sensitivity estimation. Estimation of the key-properties of a new polymer. Chapter 8. Tg-values of Polymers with Double Bonds in the Mainchain and Tg-values of Non-Polar Polymers with Sidechains
. BR with a high 1,4 trans content. BR with a high syndiotactic 1,2 BR content. Experimental IR systems. A Tg/structure correlation for non-polar polymer systems with sidechains. Chapter 9. Characterisation of Polyketone Polymer Systems by TA Techniques
. PK copolymer and PK terpolymer. The Tm(o)- and Hf(max.)-values of PK copolymer. Alpha- and beta-crystallinity in PK copolymer. Alpha- and beta-crystallinity in PK copolymer after a common processing procedure. Alpha- and beta-crystallinity in PK terpolymers. Amorphous phase transition effects. Ageing and moisture absorption effects. Determination of the Tg-value of PK terpolymer by DSC. The l.e.c. of long glass fibre reinforced PK terpolymers. The repeatability of the l.e.c. determination on PK terpolymer systems. The influence of moisture on the dielectric properties of PK terpolymer. The frequency dependency of the dielectric properties of PK terpolymer. The specific volume resistivity determination of PK terpolymer. Survey of PK terpolymer thermal analytical characterisation results. Chapter 10. Thermo-Analytical Case Studies
. Effect of the presence of a solvent during the cure of a thermoharding system. Thermal transitions of a liquid crystalline polymer. The optimal crystallisation temperature of diphenylolmethane. The dynamic stiffness of ultra-high molecular weight polypropylene in its melt. The effect of an anti-static additive on the volume resistivity of a polystyrene foam. The dielectric constant of polyethylene foil. The resistivity of epoxy based moulding powder systems during immersion in hot water. Determination of the composition of a car-tyre rubber. The thermal stability of ABS. Thermo-analytical characterisation of a maize based, 'green' polymer. Index