HIGH HEAT AMORPHOUS THERMOPLASTIC POLYIMIDE

Transcription

1 HIGH HEAT AMORPHOUS THERMOPLASTIC POLYIMIDE Steven J. Montgomery, Ph.D. Daniel Lowery Michael Donovan +, Ph.D. High Performance Polymers SABIC Innovative Plastics Mt.Vernon, IN, USA + Currently at AMCOL Research and Development, Arlington Heights, IL

2 2 Extem* XH10x5 Resin Overview EXTEM XH10x5 Resin is an unfilled, thermoplastic polyimide (TPI) offering elevated temperature performance, lead-free solderability. Versatile Portfolio: compatible with numerous amorphous & semi-crystalline resins Attributes: Mechanical Properties Highest strength & creep resistance within the HPP Resin portfolio over broad temperature range; Long term heat aging Lead free solder capability in unfilled and filled grades, ~260ºC, high RH Tensile strength of die cast aluminum at 200 C RTI testing underway expect similar to Ultem resins, ~170 C Dimensional Stability Improved dimensional stability under load vs Ultem resin to 250 C Chemical Resistance Similar to Ultem 1xxx resins Large test matrix underway for targeted markets & chemicals Inherent Flame Retardance UL mm Physical & Processing 10-20% higher flow than Ultem resin with melt temperatures ~ C Desiccant drying recommended & Melt C Injection moldable, sheet & film extrusion, and stockshapes (thick-walled) extrusion Possible Benefits: High flow amorphous thermoplastic resin with a glass transition of 267 C Better Capability to fill thin-wall, complex, miniaturized parts 50% stronger at 170 C than Ultem* resin Inherent flame resistance, high LOI Metalizability/reflectivity similar to Ultem resin; no base coat required Transparent to most visible & near IR wavelengths Transparent, dark amber in color Typical Markets Semicon. Wafer Handling Chip Trays Test Sockets E&E Military, Aerospace Connectors LED Substrates FO Lenses & Connectors Automotive Projector Reflectors Misc. Under Hood Example Applications: LED reflector Defense connector Semicon processing components Stockshape extruded & machined parts Next Generation: Complete broad design space of blends and fillers Food contact, water potability, bio-compatibility ~ 2009 * Trademark of SABIC Innovative Plastics IP BV

3 3 Extem* XH10x5 Resin Overview EXTEM XH10x5 Resin is an unfilled, thermoplastic polyimide (TPI) offering elevated temperature performance, lead-free solderability. Versatile Portfolio: compatible with numerous amorphous & semi-crystalline resins Attributes: Mechanical Properties Highest strength & creep resistance within the HPP Resin portfolio over broad temperature range; Long term heat aging Lead free solder capability in unfilled and filled grades, ~260ºC, high RH Tensile strength of die cast aluminum at 200 C RTI testing underway expect similar to Ultem resins, ~170 C Dimensional Stability Improved dimensional stability under load vs Ultem resin to 250 C Chemical Resistance Similar to Ultem 1xxx resins Large test matrix underway for targeted markets & chemicals Inherent Flame Retardance UL mm Physical & Processing 10-20% higher flow than Ultem resin with melt temperatures ~ C Desiccant drying recommended & Melt C Injection moldable, sheet & film extrusion, and stockshapes (thick-walled) extrusion Possible Benefits: High flow amorphous thermoplastic resin with a glass transition of 267 C Better Capability to fill thin-wall, complex, miniaturized parts 50% stronger at 170 C than Ultem* resin Inherent flame resistance, high LOI Metalizability/reflectivity similar to Ultem resin; no base coat required Transparent to most visible & near IR wavelengths Transparent, dark amber in color Typical Markets Semicon. Wafer Handling Chip Trays Test Sockets E&E Military, Aerospace Connectors LED Substrates FO Lenses & Connectors Automotive Projector Reflectors Misc. Under Hood Example Applications: LED reflector Defense connector Semicon processing components Stockshape extruded & machined parts STRENGTH & STIFFNESS PROPERTY RETENTION AT HIGH TEMP HIGH MELT FLOW * Trademark of SABIC Innovative Plastics IP BV Next Generation: Complete broad design space of blends and fillers Food contact, water potability, bio-compatibility ~ 2009

4 4 High Performance Polymers Performance & ASP ($) Ultra High Performance High Performance Polymers Engineering Plastics Commodity Plastics High Perf. Amorphous: Modulus at elevated temperature Dimensional stability Creep resistance ABS PPO PS PBI PI PAI PPSU PEI PSU PC Amorphous Heat PEEK LCP PPS PA POM PP PE Crystalline Amorphous PBI PI PAI EXTEM Resins PES HH PC PEI PPSU PSU Ultra High Performance: High temp. load bearing Low & stable CTE. PEEK Typically requires imidization step High Perf. Crystalline: Continuous use temp. PA46 Chemical resistance PPS PPA Wear resistance PTFE LCP Crystalline Chemical Resistance AS-MOLDED Ultra-High Performance with True Thermoplastic Melt Processability

5 5 Examples of Commercial Polyimides Kapton, Apical Solvent Cast Films Vespel Direct Formed Stockshapes Tg > 360ºC Tm ND (25-50% crystallinity in Vespel) Thermoset-like behavior Aurum ~ Tg ~ 250ºC Tm ~ 380ºC Post-molding Annealing Required to Crystallize Ultem* Resin Polyetherimide (PEI) Tg ~ 217ºC Amorphous Thermoplastic Trademarks of DuPont, Kaneka Texas Corp., ~ Mitsui Chemicals & * SABIC Innovative Plastics IP BV

6 6 Thermoplastic Polyimides (TPIs) at SABIC Innovative Plastics U.S. Europe Extem Resin Properties T o g C 340 Heat...plus Ultem Resin Ultem Siltem 5xxx, 6xxx Ultem Resin Extem Resin Ultem Capacity Expansion Enables Extem TPIs - Portfolio of Products - Tailored Properties New Monomers New High Heat Backbones & Blends Extem UH Extem XH Ultem XH6050 Chem. Res. Load Bearing Modulus, Strength, & Flow 220 Ultem 5000 Ultem 1000/1010 Pilot Semi-works Spain 200

7 7 Extem Resin Portfolio Overview Extem Resin Features all families True thermoplastic melt processability with ultra-high performance as molded Processable using high temperature injection molding equipment and conventional drying Potential in film & profile extrusion, thermoforming, stock shapes & blow molding applications Exceptional Dimensional Stability High strength, stiffness and creep resistance at elevated temperatures Inherent Flame Retardancy Outstanding Flame Smoke & Toxicity High Limiting Oxygen Index

8 8 Extem Resin Portfolio Overview- Extem UH and Extem XH Extem UH Family Glass Transition up to 311 C (592 F) Modulus retention over broad thermal range -40 C to 280ºC Extreme amorphous chemical resistance Exceptional high temperature load bearing performance Extem XH Family Glass Transition up to 267 C (513 F) Enhanced creep and strength performance at elevated temperatures Tensile strength comparable to die cast aluminum at 200 C (392 F) Approximately 50% stronger at 170 C than Ultem* resin Better capability to fill thinwall, complex, miniaturized parts Offers potential lead free solderable solutions

9 9 Extem XH Resin Product Tree EXTEM Thermoplastic Polyimide (TPI) Resin Product Family Filler Type Flow Extem XH Series Unfilled Glass Filled Mineral Filled Carbon Filled Standard Flow High Flow High Flow Standard Flow Standard Flow 66 psi/0.45mpa 250 C (482 F) 250 C (482 F) 250 C (482 F) >250 C (482 F) 257 C (495 F) Filler % 10-20% Grade Name XH1005 XH1015 AUT250 (M)** **250 C haze onset temperature Underdevelop ment in 08 30% XH2315 M= Optimized mold release for metallized reflectors

10 Unit EXTEM XH1005 ULTEM XH6050 ULTEM MECHANICAL Tensile Modulus MPa Datasheet Properties Tensile Stress, Yield % Tensile Elongation, Yield MPa Flexural Modulus MPa Flexural Stress MPa IMPACT Izod Impact, U, 23ºC J/m 1975 No Break 1335 Izod Impact, RN, 23ºC J/m Izod Impact, N, 23ºC J/m THERMAL Glass Transition Temp (Tg) CTE, 23ºC-150ºC, flow Vicat Softening Temp. Rate B HDT, 0.45 MPa, 3.2 mm HDT, 1.82 MPa, 3.2 mm ºC 1/ºC ºC ºC ºC E E E Extends the HPP Portfolio of Materials into Higher Heat Applications PHYSICAL MFR, 367ºC, 6.7 kgf (U ºC) g/10m Water Abs., Eq 23ºC % Moisture Abs., 50% RH, 23ºC % Density g/cc FLAME PERFORMANCE UL94, V0 mm OSU, 2 Min HR/Peak HR kw/m2 3/41 11/46 34/62 LOI %

11 11 High Heat Performance- DMA Modulus (MPa) Extem XH1005 Ultem XH6050 Ultem 1000 PEEK Temperature (C) EXTEM XH1005 Retains High Modulus to Temperatures in Excess of 240ºC

12 12 High Heat Performance- Tensile Strength Retention 120 Tensile Strength (MPa) Ex t e m X H P EI P ES P EEK 23 C 170 C EXTEM XH1005 Retains > 60% Tensile Strength at 170ºC (TS > 60MPa)

13 13 High Heat Performance- Specific Strength vs. Cast Aluminum 80 Aluminum/EXTEM XH Comparison Specific Tensile Strength Specific Tensile Strength (MPa cm 3 /g) EXTEM XH1005 Aluminum 6063-T5 Aluminum 1100-H Temp (deg C) Superior Specific Tensile Strength to Cast Aluminum at ~ 200ºC

14 14 High Heat Performance- Strength vs. Cast Aluminum Aluminum/EXTEM XH Comparison Tensile Strength Tensile Strength (MPa) EXTEM XH1005 Aluminum 6063-T5 Aluminum 1100-H Temp (deg C) Comparable Tensile Strength to Cast Aluminum at ~ 200ºC

15 15 High Heat Performance- Creep Creep Strain at 20MPa (100 hrs.) 2.5 ULTEM ULTEM 6000 EXTEM XH1005 Strain (%) Temperature (C)

16 16 Melt Processability- Capillary Rheometry EXTEM XH1005 (390C) Apparent Viscosity (Pa-s) 1000 ULTEM XH6050 (390C) EXTEM XH1015 (390C) EXTEM XH1005 (410C) ULTEM XH6050 (410C) EXTEM XH1015 (410C) Shear Rate (1/sec) EXTEM XH/XH 6050 Capillary Rheometry Comparison

17 17 Melt Processability- Capillary Rheometry EXTEM XH1005 (390C) Apparent Viscosity (Pa-s) 1000 ULTEM 1000 (365C) EXTEM XH1015 (390C) ULTEM 1000 (390C) EXTEM XH1005 (410C) EXTEM XH1015 (410C) Shear Rate (1/sec) EXTEM XH/ULTEM 1000 Capillary Rheometry Comparison

18 18 Melt Processability- Capillary Rheometry ULTEM 1000 (365C) Apparent Viscosity (Pa-s) 1000 ULTEM 1010 (365 C) EXTEM XH1005 (410C) EXTEM XH1015 (410C) Shear Rate (1/sec) Capillary Rheometry Comparison Temperature ~ T g + 145ºC

19 19 Melt Processability- EXTEM XH Grade Spiral Flow Comparison 14.5 MPa Pressure 204ºC Mold Temperature Flow Length (mm) XH1015 3mm XH1005 3mm XH mm XH mm XH mm XH mm Temperature ( C)

20 Melt Processability- EXTEM XH1005 Spiral Flow Analysis Spiral Flow Extem* XH1005 (3 mm) 500 Flowlength (mm) C 400 C 390 C injection pressure (Bar) flow length (mm) Spiral Flow Extem* XH1005 (2.3 mm) C 400 C C Flowlength (mm) Spiral Flow Extem* XH1005 (1.5 mm) 413 C 390 C 400 C C Injection pressure (Bar) Injection pressure (Bar)

21 21 Metallizability for Reflector Applications Directly Metallizable Without Surface Treatment or Primer Coating Inherently Strong Metal Adhesion High Haze Onset Temperature High NIR Transmission for Good Heat Dissipation Grade in Development for LED Substrates Applications T% Vs. Wavelength Haze Onset Temperature (C) Non-Annealed Annealed 1010 Tg = 217ºC XH6050 Tg = 247ºC EXTEM XH Tg = 267ºC T% ULTEM 1010 ULTEM XH6050 EXTEM XH Visible Wavelength (NM) Near-Infrared (NIR)

22 22 Extem Resin Drying Recommendations Requirements Closed Loop, Dehumidifying, Recirculating hot air hopper. Dryer conveying equipment recommended to minimize moisture exposure After-cooler location (not shown) After-cooler highly recommended Drying Conditions: 350 F (177 C) for 6-8 hours Moisture content < 0.02% Air Flow : 1 CFM per lb of resin per hour Dew point of Air -20 F to -40 F (hopper inlet); (-29 C to -40 C) Do not dry in excess of 24 hours Minimize resin in feed hopper Do not rely 100% on Dewpoint Meter üthe Most Neglected Part of the Molding Process! Typical Dryer Setup Thermocouple & Dewpoint Monitor Drying is Critical in Successfully Processing Extem Resins! RE-absorption of Water Occurs Quickly

23 23 Extem XH Resin - Processing Guidelines Summary Maximum Moisture Content % 0.02 Drying Temperature C ( F) 175 (347) Drying Time (Minimum) Hrs 6 Drying Time (Cumulative) Hrs 24 Melt Temperature C ( F) ( ) Nozzle Temperature C ( F) (707-61) Front - Zone 3 Temperature C ( F) ( ) Middle Zone 2 Temperature C ( F) ( ) Rear - Zone 1 Temperature C ( F) ( ) Mold Temperature C ( F) ( ) Back Pressure bar 3-5 Screw Speed rpm Shot to Cylinder Size % Vent Depth mm Process Capability: Minimal equipment investment Able to leverage existing mold assets Increased productivity via reduced cycle time Reduced scrap fully recyclable CRITICAL SUCCESS FACTORS: Ramp-up barrel temperature from rear zone to nozzle. Avoid pin gates. Use 40-70% of barrel capacity per cycle to reduce residence time Use low shear screw design to minimize shear Use high heat rated (ceramic) heater bands Minimize back pressure & do not use decompression/suckback (causes splay) Slow injection speed (e.g., mm/sec) is better for part appearance. Higher injections speeds give higher gloss, but watch for shear induced splay Purge using Ultem* 1000 resins Process development assistance available via PPDC and Field Tech Service

24 24 Extem Resin Regrind Study Virgin vs. 50% Regrind, Three Passes 100% XH % XH1005, pass 1 50% XH1005, pass 2 50% XH1005, pass 3 Tensile Stress, yield, 5 mm/min MPa Tensile Elongation, yield, 5 mm/min % Tensile Modulus, 5 mm/min MPa Flex Stress, yield, 1.3 mm/min, 50 mm MPa Flex Modulus, 1.3 mm/min, 50 mm MPa Izod Impact, notched 23C, 2 lb J/m Izod Impact, Unnotched 23C, 5 lb J/m 367C, 6.7 kg gm/10min Melt 400 oc, 5000s Extem Regrind Demonstrates Excellent Recyclability & Property Retention

25 25 Markets Hard Disk Drives Electrical Healthcare Aerospace & Transportation Defense Telecommunications / Satellites Consumer Automotive Under the Hood Automotive Lighting Wire & Coatings High Performance Films

26 26 Extem* XH10x5 Resin Overview EXTEM XH10x5 Resin is an unfilled, thermoplastic polyimide (TPI) offering elevated temperature performance, lead-free solderability. Versatile Portfolio: compatible with numerous amorphous & semi-crystalline resins Attributes: Mechanical Properties Highest strength & creep resistance within the HPP Resin portfolio over broad temperature range; Long term heat aging Lead free solder capability in unfilled and filled grades, ~260ºC, high RH Tensile strength of die cast aluminum at 200 C RTI testing underway expect similar to Ultem resins, ~170 C Dimensional Stability Improved dimensional stability under load vs Ultem resin to 250 C Chemical Resistance Similar to Ultem 1xxx resins Large test matrix underway for targeted markets & chemicals Inherent Flame Retardance UL mm Physical & Processing 10-20% higher flow than Ultem resin with melt temperatures ~ C Desiccant drying recommended & Melt C Injection moldable, sheet & film extrusion, and stockshapes (thick-walled) extrusion Possible Benefits: High flow amorphous thermoplastic resin with a glass transition of 267 C Better Capability to fill thin-wall, complex, miniaturized parts 50% stronger at 170 C than Ultem* resin Inherent flame resistance, high LOI Metalizability/reflectivity similar to Ultem resin; no base coat required Transparent to most visible & near IR wavelengths Transparent, dark amber in color Typical Markets Semicon. Wafer Handling Chip Trays Test Sockets E&E Military, Aerospace Connectors LED Substrates FO Lenses & Connectors Automotive Projector Reflectors Misc. Under Hood Example Applications: LED reflector Defense connector Semicon processing components Stockshape extruded & machined parts STRENGTH & STIFFNESS PROPERTY RETENTION AT HIGH TEMP HIGH MELT FLOW * Trademark of SABIC Innovative Plastics IP BV Next Generation: Complete broad design space of blends and fillers Food contact, water potability, bio-compatibility ~ 2009

27 27 ACKNOWLEDGEMENTS Colleagues at SABIC Innovative Plastics: HPP Product Technology HPP Process Technology HPP Product Management For Sample Requests and Pricing Information Contact: Rob Costella EXTEM Global Product Manager

28 28 Disclaimer: Disclaimer for product literature and pitches: THE MATERIALS, PRODUCTS AND SERVICES OF SABIC INNOVATIVE PLASTICS HOLDING BV, ITS SUBSIDIARIES AND AFFILIATES ( SELLER ), ARE SOLD SUBJECT TO SELLER S STANDARD CONDITIONS OF SALE, WHICH CAN BE FOUND AT AND ARE AVAILABLE UPON REQUEST. ALTHOUGH ANY INFORMATION OR RECOMMENDATION CONTAINED HEREIN IS GIVEN IN GOOD FAITH, SELLER MAKES NO WARRANTY OR GUARANTEE, EXPRESS OR IMPLIED, (i) THAT THE RESULTS DESCRIBED HEREIN WILL BE OBTAINED UNDER END-USE CONDITIONS, OR (ii) AS TO THE EFFECTIVENESS OR SAFETY OF ANY DESIGN INCORPORATING SELLER S PRODUCTS, SERVICES OR RECOMMENDATIONS. EXCEPT AS PROVIDED IN SELLER S STANDARD CONDITIONS OF SALE, SELLER SHALL NOT BE RESPONSIBLE FOR ANY LOSS RESULTING FROM ANY USE OF ITS PRODUCTS OR SERVICES DESCRIBED HEREIN. Each user is responsible for making its own determination as to the suitability of Seller s products, services or recommendations for the user s particular use through appropriate end-use testing and analysis. Nothing in any document or oral statement shall be deemed to alter or waive any provision of Seller s Standard Conditions of Sale or this Disclaimer, unless it is specifically agreed to in a writing signed by Seller. No statement by Seller concerning a possible use of any product, service or design is intended, or should be construed, to grant any license under any patent or other intellectual property right of Seller or as a recommendation for the use of such product, service or design in a manner that infringes any patent or other intellectual property right. SABIC Innovative Plastics is a trademark of Sabic Holding Europe BV *Trademark of SABIC Innovative Plastics IP BV Cycolac, Cycoloy, Extem, Geloy, Lexan, Lexan SLX, Lexan EXL, Noryl, Ultem, Valox, Verton, Visualfx, Xenoy, Xylex and LNP are trademarks of SABIC Innovative Plastics IP BV.