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Med-Tech Innovation Materials


Table I: Guidance on materials factors for designers and failure investigation of medical devices Polymer materials history


Batch-to-batch and other variations leading to problems/ failures


Molecular weight variation


Composition variation for copolymers


Supplied materials characterisation, including raw materials made from polymerisation, post compounding process to make pellets to be used for medical device manufacturers


Crystal structures, including short and long range crystals and crystallinity for semi-crystalline polymers


Viscoelastic property variation


Spherulite crystal phase variation


Nano/micro structure variation


Process ability variation


Changes in production and process, equipment (maintenance schedule, inspection, adjustment), manufacturing material and personnel


Product failure investigation: here product means any products from start to the end of a process. This is because a medical device can fail at any stage of the manufacturing process; each stage can potentially cause polymer structure changes and therefore potentially lead to a defect(s) causing finished device failure before shipping and afterwards.


Material changes during manufacturing: Variation can lead to changes in nano/microstructure and mechanical properties and therefore affect the performance of the medical device


Tests/methods for materials characterisation


Gel permeation chromatography


Fourier transform infrared spectroscopy (FTIR)


Wide/small angle X-ray scattering (WAXS/SAXS)


Differential scanning calorimeter (DSC)


Dynamic mechanical thermal analysis (DMTA)


Cross polarisation optical microscope


Scanning electron microscopy/ Transmission electron microscopy (SEM/TEM)


Rheology: Cone plate or capillary rheometer


Update SOPs, equipment inspection, measuring and test, training record


Surface analysis


Important parameters/factors to know


Number average (Mn); weight average (Mw)


Chemical finger print


Nano crystal cell dimension; long range lamellae


Glass transition temperature (Tg) Melting and crystallisation temperatures (Tm/Tc)


Viscoelastic properties and dynamic modulus as a function of temperatures and Tg


Spherulite crystal structure


Different nano/micro structure/ phases arrangement within polymer matrix


Process ability: Viscosity variation as function of shear rates and/or temperature


What, why, when changes are made: Calibrations, calibration standards, calibration records


X-ray photoelectron spectroscopy (XPS): Quantitative chemical mapping of materials


Secondary ion mass spectrometry (SIMS) and Time-of-flight surface mass spectrometry (ToFSIMS)


Surface topography: 3D non-contact profiling


Bulk mechanical property analysis, including films and fibres and other geometries


SEM and 3D SEM analysis Mechanical test such as tensile deformation to failure to evaluate basic mechanical properties


Fracture mechanics to evaluate fracture toughness


Viscoelastic properties: Creep/stress relaxation variation as function of time and temperature


Internal nano and microstructure analysis


WAXS/SAXS to evaluate crystallinity and long range changes


SEM/TEM: Nano/micro structure/ phases changes caused by variation of manufacturing


Thermal analysis


DSC for evaluation of manufacturing caused variation, including glass transition temperature and melting temperature for semi-crystalline polymers


DMTA for evaluation of manufacturing caused variation of viscoelastic and mechanical properties as function of temperature


Continued... www.med-techinnovation.com November/December 2011 ¦ 31


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