Polymers and Rubbers Application Compendium

Importance of the topic

Advanced analytical techniques are critical for understanding and controlling the properties of polymeric materials, rubber products and advanced low-k dielectrics. Accurate testing of composition, morphology, mechanical strength and electrical behavior under real-world conditions ensures quality control, optimizes performance and supports innovation in materials research and industrial production.

Objectives and overview of the studies

Agilent’s comprehensive materials testing and research platform integrates multiple instruments and methods to:

• Quantitatively characterize polymer additives, copolymer ratios and contaminant identification via FTIR spectroscopy
• Map nanoscale electrical and mechanical properties using multi-frequency AFM and Kelvin probe force microscopy
• Measure hardness, modulus and scratching resistance of thin films and coatings by instrumented nanoindentation
• Monitor structural transformations of polymer assemblies under varied environmental atmospheres with environmental AFM
• Evaluate mechanical performance of low-k dielectric films at elevated temperatures for semiconductor applications

Methodology and instrumentation used

• Fourier Transform Infrared (FTIR) spectroscopy with ATR sampling for quantitative analysis of polymer blends and additives, using Cary series spectrometers and DialPath/TumblIR cells
• Atomic Force Microscopy (AFM) in contact, amplitude-modulation (AM) and frequency-modulation (FM) modes, augmented by MAC III multi-lock-in accessory for probing topography, phase, surface potential and dielectric response
• Single-pass Kelvin Force Microscopy (KFM) for simultaneous mapping of surface potential and topography in the intermittent-contact regime
• Instrumented nanoindentation and continuous stiffness measurement (CSM) for depth-profiled elastic modulus and hardness, along with ramp-load scratch tests for coating adhesion and wear resistance
• Environmental AFM chambers enabling controlled humidity and solvent vapor exposure to study swelling, self-assembly and film morphology
• Elevated-temperature indentation equipped with a hot-stage and inert-gas purging for mechanical testing up to 350 °C

Main results and discussion

• FTIR-ATR methods achieved linear, sensitive quantification of styrene in SBR, vinyl acetate in PEVA, copolymer ratios, and antioxidant levels with detection limits below 0.1 wt %
• AFM-based KFM resolved surface potential differences of 10 mV at nanometer spatial scales, distinguishing polymer domains, semiconductor dopant regions and contaminant particles
• Multi-frequency detection (AM-AM, AM-FM, FM-AM) in Kelvin force microscopy revealed enhanced sensitivity and higher resolution of electrostatic features when using FM detection for surface potential nulling
• Nanoindentation on coated and uncoated polymer films demonstrated Young’s modulus and hardness up to 10 µm depth, with clear differentiation of hard coatings versus underlying substrates, and scratch tests showed critical loads increased from <1 mN to >7 mN
• Environmental imaging uncovered humidity-induced conformational changes in block copolymers, self-assembly transformations of semifluorinated alkanes, and nanoscale pore structures in Nafion® membranes via phase and surface potential contrast
• Elevated-temperature testing up to 100 °C on cellulose films maintained consistent modulus (≈ 3 GPa) and hardness, confirming suitability for display screen applications

Benefits and practical applications of the methods

• Quality assurance and process control in polymer manufacturing, rubber compounding and electronics encapsulation
• Identification of polymer contaminants (e.g. sealing materials, grease, fuel additives) in production and failure analysis
• In-line verification of low-k dielectric properties for semiconductor interconnect reliability
• Surface engineering validation for scratch-resistant coatings on consumer electronics
• Nanoscale insight into self-assembly and morphology of block copolymers for nanofabrication

Future trends and potential uses

• Expanded adoption of FM-based multi-frequency AFM and KFM modes for atomic-scale electrical mapping under ambient and liquid conditions
• Integration of environmental control with in situ mechanical-electrical testing for real-time observation of stimuli-responsive materials
• Advanced substrate-compensation models for accurate nanoindentation of ultrathin films and 2D materials
• Coupling AFM-based compositional mapping with machine learning for automated defect detection in high-throughput manufacturing

Conclusion

Agilent’s portfolio of FTIR spectroscopy, advanced AFM, KFM, nanoindentation and environmental microscopy provides a versatile toolkit for comprehensive materials characterization from molecular to microscale. The methods deliver quantitative data on composition, mechanical strength, wear resistance, electrical properties and environmental responsiveness—critical parameters for research, quality control and product development across polymers, rubbers, low-k dielectrics and emerging nanomaterials.

References

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