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David Vroom Consultant
Development of Advanced Development of Advanced Development of Advanced Development of Advanced CrossCrossCrossCross----linking Materialslinking Materialslinking Materialslinking Materials
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Scope of the PresentationScope of the PresentationScope of the PresentationScope of the Presentation
Materials designed for radiation processing• Cross-linking of Polymers – Industrial
applications- wire and cable insulation - elastic memory products- circuit protection devices - positive temperature coefficient (PTC)
heaters
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Scope of the PresentationScope of the PresentationScope of the PresentationScope of the Presentation
• Industry oriented – non-academic- complex, proprietary formulations
• No trade secrets, formulations• Product oriented
- market pull• Emphasis on e-beam irradiated
materials
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TodayTodayTodayToday’’’’s Split Markets Split Markets Split Markets Split Market
• High performance / high cost / niche- aerospace - defense- marine - ferries- medical- mass transit- energy generation / distribution- telecommunications – outside plant- circuit protection - telecommunications - industrial heating
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TodayTodayTodayToday’’’’s Split Markets Split Markets Split Markets Split Market
• Required performance / low cost / pseudo commodity- automotive- commercial electronics- commercial general- circuit protection – batteries - non-industrial heating
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TodayTodayTodayToday’’’’s markets markets markets market
• Green- bio-degradable- recyclable formulations- use of recycled materials
• RoHS- reduce / eliminate heavy metals- lead free (soldering)
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TodayTodayTodayToday’’’’s markets markets markets market
• Higher operating / maximum temperatures
• Small dimensions• Light weight• More aggressive solvents• Extended life
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TodayTodayTodayToday’’’’s Realitys Realitys Realitys Reality
• Reformulation- raw materials obsolescence
- edge materials- changing regulations- challenge all components availability
• Materials allocation- fluoropolymers
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High Performance MaterialsHigh Performance MaterialsHigh Performance MaterialsHigh Performance Materials
• Higher cost acceptable• High quality• Meet or beat the spec.• Higher operating temperatures
- lead free soldering applications- engine compartments
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High Performance MaterialsHigh Performance MaterialsHigh Performance MaterialsHigh Performance Materials
• Superior mechanical properties- defense applications
• Superior chemical properties- NBC (nuclear, biological, chemical)
• Acceptable manufacturability• Acceptable delivery – longer lead times• Generally lower volumes
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Acceptable Performance Acceptable Performance Acceptable Performance Acceptable Performance MaterialsMaterialsMaterialsMaterials• Lowest possible cost or lower• High quality• Meet the spec.• Appropriate operating temperature• Appropriate mechanical properties• Appropriate chemical resistance
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Acceptable Performance Acceptable Performance Acceptable Performance Acceptable Performance MaterialsMaterialsMaterialsMaterials• Environmentally acceptable
- RoHS, halogen free• Superior manufacturability• Superior delivery – off-the-shelf,
scheduled deliveries• Generally higher volumes
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Materials CharacteristicsMaterials CharacteristicsMaterials CharacteristicsMaterials Characteristics
High performance and acceptable performance crosslink-able polymeric
materials are complex and require significant development.
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Materials Development ProcessMaterials Development ProcessMaterials Development ProcessMaterials Development Process
• Needs / specification from customer• Product design – specification
refinement• Formulation – choose polymer(s),
modifier(s), additives – iterative process, pass the tests
• Compounding – scaling issues• Manufacturability
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Choosing the right componentsChoosing the right componentsChoosing the right componentsChoosing the right components
• Market needs drive choice of components- low cost – polyolefin co-polymers- high temperature – fluoropolymers, - high expansion ratio – highly branched
polyolefins- oil resistance – fluoropolymers- chemical resistance – fluoropolymers,
fluoroelastomers, polyesters
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Choosing the right componentsChoosing the right componentsChoosing the right componentsChoosing the right components
• Market needs drive the choice of components- abrasion resistance – fluoropolymers, - cut through resistance - nylons- lubricity – fluoropolymers- biocompatibility - flame retardants – brominated
compounds, red phosphorous, water releasing compounds (Mg(OH)2, Al2O3
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Choosing the right componentsChoosing the right componentsChoosing the right componentsChoosing the right components
• Chemistry helps guide components choice- compatibility of components- cross-linking stabilization of quasi-
compatible components- material interaction with the
environment – substrate
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Choosing the right componentsChoosing the right componentsChoosing the right componentsChoosing the right components
• Chemistry helps guide components choice- adhesive bond to jacket - substrate- crosslink / degradation dose matching
- multiple layer products- temperature matching – jacket,
adhesive- e-beam vs. Co-60 irradiation – dose
rate issues
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Commonly Used PolymersCommonly Used PolymersCommonly Used PolymersCommonly Used Polymers
Little change over the past 25 years• Polyolefins
- polyethylene – HD, LD, LLD, VL, UL- co-polymers – EMA, EBA, EVA (modifiers)
• Fluoropolymers- ETFE, PVDF, PFA/MFA,
(PTFE)
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Commonly Used PolymersCommonly Used PolymersCommonly Used PolymersCommonly Used Polymers
• Elastomers- EPDM, fluoroelastomers (modifiers)
• Polyesters – PBT, Hytrel• Nylons – 11, 12• Polyamides (adhesives)
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Additives Additives Additives Additives
List of 35 types of additives• Antioxidants• Biocides• Blowing agents
- Physical blowing agents (compressed gases, volatile liquids)
- Chemical blowing agents (solid compounds that decompose to evolve gas)
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AdditiveAdditiveAdditiveAdditive
• Conductive fillers – for PTC heaters, circuit protection devices, high voltage stress grading, EMI shielding, induction heating - carbon blacks- metal powders- ferromagnetic materials
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AdditivesAdditivesAdditivesAdditives
• Cross-linking enhancers - radiation• Cross-linking inhibitors - radiation• Chemical curing agents (peroxides)• Degradability agents (to promote bio- or
photo- degradation)• Fiber (glass, graphite, metal, etc) for
reinforcing
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AdditivesAdditivesAdditivesAdditives
• Flame retardants- Halogenated- Halogen free- Synergists
• Inert fillers (low cost)• Pigments• Recyclate additives (to boost properties
of recycled plastics)• UV stabilizers
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Meet the customer needs / specificationMarket drives choices - use temperature / maximum
temperature- flame retarded- low smoke- electrical properties- solvent resistance
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Meet the customer needs / specificationMarket drives choices - mechanical properties- installation methods / concerns- cost- weight- product size range
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Choose base polymer(s)- determines main features of material
- operating temperature range- gross mechanical and chemical properties
- effects of crystallinity – additives contained in amorphous regions only
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Choose base polymer(s)- average molecular weight
- crosslink-ability vs. melt process-ability
- molecular weight distribution- crosslink-ability vs. melt process-
ability
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Choose polymer modifiers- reduce crystallinity – important if high
additive levels required in highly crystalline materials like HD polyethylene
- increase flexibility- lower cost
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Choose polymer modifiers- compatibility of polymers and other
additives- quasi compatibility – use radiation to
lock components together - materials that are designed to absorb
and coat other materials- improve manufacturability –
processing speed, drool, clogs
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Additives- complex formulations – in excess of 10
components in some cases- high solids (non-melting) content – can
be over 50%- green anti-oxidant and flame
retardant packages - particle size – small tubing, conductive
polymers
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• Additives- green cross-linking promoters
- phasing out traditional types like tri-chlorobenzene (TCB)
- pigments – heavy metals, radiation bleaching / color change
- compatibility - bleeding
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
• One formulation may not pass all tests in product size range- cost- VW1 flame test – UL test- chemical resistance- titrate the formulation to fine tune- should look and feel the same
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Formulation ConsiderationsFormulation ConsiderationsFormulation ConsiderationsFormulation Considerations
The effects of radiation on all components must be
understood
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsHigh Performance – Energy production /
distribution – splices / terminations• Needs
- high voltage insulation – up to 69KV- acceptable shrink time- cable type specific – oil filled / solid
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsHigh Performance – Energy production /
distribution, tubing / molded parts• Needs
- moisture proof- stress grading- no arc-tracking - charring- rodent / insect proof- minimal uv degradation (30 yr. life)
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsHigh Performance – Energy production /
distribution, tubing / molded parts• Solutions
- product design- thick wall product / shrink time / dual /
multi-layer wall thermoplastic / elastomer product
- Co-60 irradiation – thick / rigid
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsHigh Performance – Energy production /
distribution, tubing / molded parts• Solutions
- polyolefin or fluoropolymer holdout layer – EPDM inner layer
- conductive additives for stress grading
- additives to eliminate arc tracking –diatomaceous earth
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsAcceptable performance – Automotive
tubing / molded parts• Needs – a demanding market
- low cost- delivery, delivery, delivery – line down
considerations- high quality- cable systems protection - moisture
sealing
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsAcceptable performance – Automotive
tubing / molded parts• Needs
- chemical resistance – brake fluids, coolants, oils, fuel
- abrasion resistance- higher temperature jackets and
adhesives
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsAcceptable performance – Automotive
tubing / molded parts• Needs
- rapid, reliable, foolproof installation- color matching - beautification - generally green
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsAcceptable performance – Automotive
tubing / molded parts• Solutions
- single and dual wall requirements- polyolefin HDPE, LDPE /
fluoropolymers based outer jacket- adhesive / blocking material inner wall
- matched to jacket and substrate
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Elastic Memory Elastic Memory Elastic Memory Elastic Memory –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials SolutionsAcceptable performance – Automotive
tubing / molded parts• Solutions
- metal filled material – induction heating sensitive additives in jacket and adhesive / blocking layers –induction heating for installation
• Reliable components supply and manufacturing process
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Circuit Protection Circuit Protection Circuit Protection Circuit Protection –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
High and acceptable performance• Needs
- Low resistance – milli-Ohms for small components
- Low cost- Smaller, smaller and smaller – battery
pack surface mounted down to 0.5 mm by 0.5 mm
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Circuit Protection Circuit Protection Circuit Protection Circuit Protection –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
High and acceptable performance• Needs
- Reliability, reliability, reliability- telecommunications - long- cell phone – two year lifetime- automotive – ten year life time
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Circuit Protection Circuit Protection Circuit Protection Circuit Protection –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
High and acceptable performance• Solutions
- PE, PE co-polymers and fluoropolymers- Carbon black most common conductive filler- New products using metal powder
conductive fillers are being introduced- Processing is as important as the material
formulation – orientation- Co-60 and e-beam processing
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Circuit Protection Circuit Protection Circuit Protection Circuit Protection –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
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PTC Heaters PTC Heaters PTC Heaters PTC Heaters –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions• Needs
- range of auto- regulating temperatures
- range of power outputs (watts/meter)- longer lengths between power points- solvent resistance- abrasion resistance, indoor / outdoor
applications
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PTC Heaters PTC Heaters PTC Heaters PTC Heaters –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions• Solutions
- Carbon black conductive filler- Olefin based heaters - 85° C shut off- PVDF based heaters - 110° C shut off- PFA / MFA based heaters - 121° C
shut off- product design – outer jackets / braids
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PTC Heaters PTC Heaters PTC Heaters PTC Heaters –––– Market Needs, Market Needs, Market Needs, Market Needs, Materials SolutionsMaterials SolutionsMaterials SolutionsMaterials Solutions
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Concluding RemarksConcluding RemarksConcluding RemarksConcluding Remarks
• Materials development market driven• Both high performance and acceptable
performance materials are complex and require significant development
• Product designers and materials formulators must work together
• Shift toward smaller product sizes, light weight and green
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Concluding RemarksConcluding RemarksConcluding RemarksConcluding Remarks
• Available number of cross-linking polymers and additives is extensive
• Compounding route is a crucial part of the development process
• Small variations in composition, compounding can result in failure to qualify
• Education / experience concerns