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Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University of Bradford, Bradford UK. IRC in Polymer Engineering, University of Bradford, Bradford UK. P S Allan, G. Greenway and P Hornsby, Wolfson Centre for Materials Processing, Brunel University, Uxbridge, UK

Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

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Page 1: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Micro-Moulding of Polymers:Process and Product Assessments

Micro-Moulding of Polymers:Process and Product Assessments

Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates,

IRC in Polymer Engineering, University of Bradford, Bradford UK.IRC in Polymer Engineering, University of Bradford, Bradford UK.

P S Allan, G. Greenway and P Hornsby,

Wolfson Centre for Materials Processing, Brunel University, Uxbridge, UK

Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates,

IRC in Polymer Engineering, University of Bradford, Bradford UK.IRC in Polymer Engineering, University of Bradford, Bradford UK.

P S Allan, G. Greenway and P Hornsby,

Wolfson Centre for Materials Processing, Brunel University, Uxbridge, UK

Page 2: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

ContentsContents

• Micromoulding • Process technology

• Results of studies at Bradford• Process dynamics• Process interaction• Product properties

• Micromoulding • Process technology

• Results of studies at Bradford• Process dynamics• Process interaction• Product properties

Page 3: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

• Purpose built micro injection process

• Servo-electric injection

• Automatic parts handling

• Clean room filtration

• Modular

Battenfeld Microsystem 50Battenfeld Microsystem 50

Page 4: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Battenfeld Microsystem 50Battenfeld Microsystem 50

Metering PistonMetering Piston

HopperHopper

Shut off valveShut off valve

Extrusion screwExtrusion screw

Heated RegionsHeated Regions Injection pistonInjection piston

Page 5: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Operation CycleOperation Cycle

Page 6: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Dynisco PCI 4011 Piezo load transducer

Dynisco PCI 4011 Piezo load transducer

Dynisco PCI 4006 piezo load transducer

Dynisco PCI 4006 piezo load transducer

The Data Acquisition SetupThe Data Acquisition Setup

Temposonics R series displacement transducer

Temposonics R series displacement transducer

J-type thermocouplesJ-type thermocouples

Page 7: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

1 Process Measurement – Data Capture

1 Process Measurement – Data Capture

Injection Pressure

Cavity Pressure

Ram Displacement

Ram Velocity

3 Temperature Channels

Injection Pressure

Cavity Pressure

Ram Displacement

Ram Velocity

3 Temperature Channels

Max sampling rate ~ 30 000HzMax sampling rate ~ 30 000Hz

Page 8: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Mould temperature investigationMould temperature investigation

Page 9: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

HypothesisHypothesis

• The high surface area to volume ratio of micro-moulded products allows rapid removal of heat from the product through the cavity wall

• Mould temperatures should be higher than those used in conventional IM to prevent premature solidification and part-filled products

• The high surface area to volume ratio of micro-moulded products allows rapid removal of heat from the product through the cavity wall

• Mould temperatures should be higher than those used in conventional IM to prevent premature solidification and part-filled products

Page 10: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Step plaque mouldingStep plaque moulding

Material: HAPEX (40% sintered hydroxyapatite HDPE matrix)

Produced by IRC in Biomaterial Science

Queen Mary and Westfield College, London

Material: HAPEX (40% sintered hydroxyapatite HDPE matrix)

Produced by IRC in Biomaterial Science

Queen Mary and Westfield College, London

Page 11: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Cavity Pressure – Hapex, step plaque

Cavity Pressure – Hapex, step plaque

80C

50C

20C

Page 12: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Product Mass – Hapex, step plaqueProduct Mass – Hapex, step plaque

0.12% variation0.12% variation

Page 13: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Mould temperature - conclusionsMould temperature - conclusions

• For products ~25mg recommended mould temperatures for standard injection moulding can be used with confidence for the Hapex material

• Further investigations to be performed at smaller length scales

• For products ~25mg recommended mould temperatures for standard injection moulding can be used with confidence for the Hapex material

• Further investigations to be performed at smaller length scales

Page 14: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

High shear rate experimentsHigh shear rate experiments

Page 15: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Calculated wall shear ratesCalculated wall shear rates

0.1 x 0.1mm

0.2 x 0.2mm

0.5 x 0.5mm

1.0 x 1.0mm

Page 16: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

In-process rheometryIn-process rheometry

• Measurements performed on a 30 tonne Cincinnatti Milacron servo-electric injection moulding machine with a custom rheometric nozzle

• Measurements performed on a 30 tonne Cincinnatti Milacron servo-electric injection moulding machine with a custom rheometric nozzle

Dynisco Pressure Transducer 435-30M

Dynisco Pressure Transducer 435-30M

Capillary dieinsertsCapillary dieinserts

0.5 x 8.0 mm0.5 x 0.25 mm

1.0 x 16 mm1.0 x 0.25 mm

ThermocoupleThermocouple

Page 17: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

High-shear capillary rheometry test resultsHigh-shear capillary rheometry test results

Page 18: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Shear heating effectsShear heating effects

Source: Anthony Bur, Steven Roth, NISTSource: Anthony Bur, Steven Roth, NIST

Page 19: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

‘Top Hat’ Cavity‘Top Hat’ Cavity

• Large diameter = 1.0mm• Small diameter = 0.5mm• Gate dimension 0.1 x 0.2mm• Material BP Rigidex 5050 HDPE

• Large diameter = 1.0mm• Small diameter = 0.5mm• Gate dimension 0.1 x 0.2mm• Material BP Rigidex 5050 HDPE

Page 20: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Molecular weight measurementMolecular weight measurement

• Sample material taken from runner system and cavity

• Gel Permeation Chromatography (GPC) analysis performed by Rapra Technology Ltd on each sample to determine molecular weight distribution

• Sample material taken from runner system and cavity

• Gel Permeation Chromatography (GPC) analysis performed by Rapra Technology Ltd on each sample to determine molecular weight distribution

Page 21: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Molecular weight distributionsMolecular weight distributions

Source: RAPRA UKSource: RAPRA UK

Page 22: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

High shear investigation - conclusions

High shear investigation - conclusions

• The process contains shear rates orders of magnitude higher than those encountered in conventional IM

• Viscosity curves behave predictably in this region

• Shear heating will be a factor• Stable materials show no sign of

degradation• Temperature sensitive materials?

• The process contains shear rates orders of magnitude higher than those encountered in conventional IM

• Viscosity curves behave predictably in this region

• Shear heating will be a factor• Stable materials show no sign of

degradation• Temperature sensitive materials?

Page 23: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replicationSurface feature replication

Page 24: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replicationSurface feature replication

• Plaque cavity 25 x 2.5 x 0.25 mm• Fabricated using micro-milling technique

• Kern machine• 0.2mm cutter at 75 000 rpm.• Left in an unpolished state.

• Plaque cavity 25 x 2.5 x 0.25 mm• Fabricated using micro-milling technique

• Kern machine• 0.2mm cutter at 75 000 rpm.• Left in an unpolished state.

Page 25: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replication - gateSurface feature replication - gate

AFM scan size 75 µm x 75 µm

Pitch of scroll marks ~ 6µm

AFM scan size 75 µm x 75 µm

Pitch of scroll marks ~ 6µm

Cavity Product

Page 26: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replication - gateSurface feature replication - gate

AFM scan size 75 µm x 75 µm AFM scan size 75 µm x 75 µm

Cavity Product

Page 27: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replication -downstreamSurface feature replication -downstream

AFM scan size 75 µm x 75 µm

Pitch of scroll marks ~ 6µm

AFM scan size 75 µm x 75 µm

Pitch of scroll marks ~ 6µm

Cavity Product

Page 28: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Surface feature replication - comments

Surface feature replication - comments

• Mould features of the order of a few µm are accurately replicated on the product assuming pressure is sufficient

• Further work to be performed to investigate the limit to which a feature is adequately moulded on a product

• Mould features of the order of a few µm are accurately replicated on the product assuming pressure is sufficient

• Further work to be performed to investigate the limit to which a feature is adequately moulded on a product

Page 29: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Morphology MeasurementMorphology Measurement

• Component sectioned using glass-knife microtomy

• Surface is etched using potassium permanganate solution to produce representative surface

• Surface imaged using microscopic technique (TEM, AFM etc)

• Component sectioned using glass-knife microtomy

• Surface is etched using potassium permanganate solution to produce representative surface

• Surface imaged using microscopic technique (TEM, AFM etc)

Surface following microtomy Surface following etching

Page 30: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Morphology Measurements - Structure Morphology Measurements - Structure

Nano-indentNano-indent

Crystal StructureCrystal Structure

Page 31: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Morphology Measurements – Spherulite size

Morphology Measurements – Spherulite size

Page 32: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Morphology VariationMorphology Variation

Line of indents 25µm separationLine of indents 25µm separation

800 µm

Page 33: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University
Page 34: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University
Page 35: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Morphology Measurements – Amorphous layer

Morphology Measurements – Amorphous layer

Page 36: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

The Rondol Micro-Injection Compounder

The Rondol Micro-Injection Compounder

Page 37: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

The Rondol Micro-Injection Compounder

The Rondol Micro-Injection Compounder

Page 38: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

The Rondol Micro-Injection Compounder

The Rondol Micro-Injection Compounder

Prism twin-screw extruderPrism twin-screw extruder

Page 39: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

The Rondol Micro-Injection Compounder

The Rondol Micro-Injection Compounder

Advantages:

• Minimise residence time of polymer in plasticising screw

• Exposure to single heating/cooling cycle

• Positive displacement allows use of low viscosity materials

Advantages:

• Minimise residence time of polymer in plasticising screw

• Exposure to single heating/cooling cycle

• Positive displacement allows use of low viscosity materials

Page 40: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

OperationOperation

Page 41: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

The Rondol Micro-Injection Compounder

The Rondol Micro-Injection Compounder

Page 42: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

Initial testingInitial testing

• It works!• Able to process low molecular weight materials• It works!• Able to process low molecular weight materials

• Dosing control can fluctuate• Toggle clamp can result in flashing• Dosing control can fluctuate• Toggle clamp can result in flashing

Page 43: Micro-Moulding of Polymers: Process and Product Assessments Dr Ben Whiteside, Dr Mike Martyn, Prof Phil Coates, IRC in Polymer Engineering, University

ExperimentalExperimental

Battenfeld Microsystem50Stepped plaque cavity

60mg total shot massHDPE 5050Injection speed – 200, 400, 600 mm/sScrew speed 40revs/mMelt temp 200CMould temp 50C

Battenfeld Microsystem50Stepped plaque cavity

60mg total shot massHDPE 5050Injection speed – 200, 400, 600 mm/sScrew speed 40revs/mMelt temp 200CMould temp 50C