Application Data Book - Polymer and Electronic Material

Importance of the Topic

Thermal analysis techniques such as DSC, TGA and DTG are essential for characterizing polymer and electronic materials by measuring transitions, decomposition kinetics and composite composition. These methods underpin quality control, materials development and safety evaluation in industries ranging from plastics and rubber to semiconductors and energy devices.

Study Objectives and Overview

This application data book presents a series of case studies illustrating how the Thermal Analysis 60 Series instruments are applied to:

• Assess heat treatment effects on crystallinity and thermal history of polymers
• Determine glass transition, melting and crystallization behavior
• Monitor decomposition and oxidation reactions, including oxygen induction time
• Quantify reinforcing fillers such as glass fiber, carbon black and quartz
• Characterize thermal behavior of electronic components and solder alloys
• Analyze battery separators and fuel cell membranes

Methodology and Instrumentation

Measurements were performed using Shimadzu thermal analyzers under controlled atmospheres:

• DSC-60 for heat flow experiments (Tg, melting, crystallization, reaction enthalpies, OIT)
• TGA-50 for thermogravimetric decomposition and filler quantification
• DTG-60 for combined TG-DTA analysis in nitrogen or air

Sample masses ranged from 2 to 24 mg. Heating rates varied from 1 to 50 °C/min, with isothermal holds applied for oxidation and reaction kinetics studies.

Main Results and Discussion

Key findings across the studies include:

• PET: Rapid cooling yields amorphous material with Tg around 78 °C, exothermic recrystallization at 137 °C and melting at 255 °C
• PEEK: Film form is noncrystalline with Tg 144.6 °C, while block form shows melting at 339.2 °C
• Nylon A and B: Melt peaks at 102–108 °C and crystallization at 147–153 °C reveal lot-to-lot variation
• PP heat treatment: Two one-hour holds at 230 °C reduce crystallinity by approximately 6%
• PE–PP blends: DSC peak areas accurately determine a 1:1 mixing ratio
• High-impact PS and PVC: Impact modifiers and plasticizer lower Tg by 7–14 °C; rapid cooling after heat treatment raises Tg by 5–7 °C
• Polyimide: Glass transition at 307.6 °C and curing exotherm at 371.4 °C shift to 314.8 °C on second heating
• Nylon 6: Melting at 222 °C and main decomposition at 447 °C, with minor dehydration below 200 °C
• Modified PPO and PET: Decomposition onset near 300–350 °C; isothermal holds quantify slow mass loss
• PE oxidation: Oxygen induction times of 78.6 min at 190 °C and 20.5 min at 200 °C
• Fluororesin: Nearly complete mass loss by 569 °C in air
• Phenol resin: Tg at 70.9 °C and condensation exotherm at 169.1 °C using high-pressure crucible
• Filler quantification: 34.2% glass fiber in PET, 28.2% carbon black in SBR, 66.2% quartz in epoxy resin
• Electronic components: Diode melting at 225–361 °C prior to decomposition; lead-free solder melts at 209–217 °C versus 182 °C for conventional Sn–Pb
• Battery separators: Polyethylene membranes exhibit melting between 130–160 °C, with enthalpy reflecting crystallinity order c > b > a
• Fuel cell film: DSC detects water cluster melting below 0 °C and free ice at 0 °C

Benefits and Practical Applications

Thermal analysis delivers rapid, quantitative insights into polymer structure, stability and additive content. This supports formulation optimization, batch consistency checks, verification of filler loading and safety assessments for electronic and energy materials.

Future Trends and Opportunities

Advances are expected in coupling thermal analysis with evolved gas analysis, high-throughput microscale calorimetry, in situ monitoring of reactive processes and integration with predictive machine-learning models for accelerated materials design.

Conclusion

The Thermal Analysis 60 Series provides a versatile toolkit for addressing diverse analytical challenges in polymer and electronic materials, enabling the extraction of critical thermal and kinetic parameters for research, quality control and product development.

Reference

Shimadzu Corporation Thermal Analysis 60 Series Application Data Book Polymer and Electronic Material C160-E010B First Edition November 2012 3655-01505-PDFIK