Injection Molding LSR Parts with Micro and Nanostructured Surfaces. SmartManufacturingSeries.com

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1 Injection Molding LSR Parts with Micro and Nanostructured Surfaces SmartManufacturingSeries.com

2 Liquid Silicone Rubber (LSR) Two-component addition cure system Pt catalyst fast ( s) cure Compared 6-12 min. cure for gum-based silicones Relatively fluid Shore A Hardness Viscosity, Pa-s Density, kg/m Biologically insert Wide temperature range: -75 to 315 C

3 Why LSR Micro/Nanofeatures? Cast polydimethylsiloxane (PDMS) widely used for research Limited feature dimensions and low aspect ratios 1-4 Critical aspect ratio depends on modulus 4 AR critical 0.57E 1/ 3 1/ 6 1/12 s d (1 ) LSR aspect ratios 70% higher than PDMS 5 1/ 3 s 1/ 2 1 Kwon et al., Journal of Nanoscience, Article ID (2016); 2 Delamarcheet al., Advanced Materials, 9, (1997); 3 Shao et al., Sensors and Actuators A: Physical, 178, (2012); 4 Chen et al., Sensors and Actuators A: Physical, 189, (2013); 5 Pokroy et al., Advanced Materials, 21, (2009)

4 Limited Injection Molding of Microstructured LSR Surfaces Diameter, m Aspect Ratio Spacing Ratio Processing Conditions Height Ratio Zhang et al :1 0.5: Kaitainen et al :1 0.8:1, 4: Hopmann et al and :1 to 1.5:1 1.3:1, 1.6:1 T mold,t melt, v inj -- Aspect Ratio: Height/Diameter; Spacing Ratio: Spacing/Diameter; Height Ratio: Part Feature Height/Tool Feature Depth 1 Zhang et al., Proc. of the 15th Int. Conference on Metrology and Properties of Engineering Surfaces, ASPE (2015); 2 Kaitainenet al., Sensors and Actuators A: Physical (2014); 3 Hopmann et al., Silicon (2013)

5 This Work Investigate injection molding of microstructured surfaces from LSR Effect of tooling feature sizes Effect of processing conditions Mold temperature In-mold curing time Shot size Vacuum venting Compare failure mechanisms of LSR to PDMS

6 Experimental Approach LSR Elastosil LR 3003/50 (Wacker) E = 9.9 MPa E a = kj/mol Injection molded using Battenfeld BA 400CDC Steel mold with silicon tooling insert PDMS control Sylgard 184 (Dow Corning) Mixed in 10:1 ratio Mixture degassed for 30 min Cast under vacuum Temperature: ~20 C Time: 48 h Recommended Molding Conditions T melt : 25 C T mold : C t curing : 5-8 s/mm

7 Mounting Tooling Inserts 35 mm 15 mm 10 mm 50 mm Sprue PTFE Tool steel Glass-fiber reinforced cloth tape Silicon wafer

8 Characterization of Structured Surfaces Scanning electron microscopy JEOL JSM-7401F Diameter ratio (DR) DR Height ratio (HR) D D h HR d part tooling part tooling feature feature feature feature

9 1: Microstructured Surfaces Tooling Diameter, Resultant µm Aspect Ratio Spacing Ratio P P P Anti-stiction coating: perfluorooctyl-trichlorosilane

10 Processing Conditions Study 1 Study 2 Study 3 Study 4 T melt, C ~20 C - due to water cooled barrel T mold, C 160, 185, t cure, s 10, 25, Post Cure 4 h at 200 C Inj. Rate, mm/s 25 x 10-3 mm 3 /s Holding 14 MPa for 30 s Vacuum Yes No Yes Yes Shot Size, % , 96, Switchover Method Position Position Position Pressure Tooling All P50, P8 P115 P50

11 Result: Excellent Feature Replication P115 P50 P8 200 µm 200 µm 20 µm 200 µm 200 µm 20 µm DR = 1.01 ± 0.01 HR = 1.05 ± 0.01 DR = 1.01 ± 0.01 HR = 1.02 ± 0.01 DR = 1.01 ± 0.01 HR = 1.02 ± 0.02

12 Clear Replication of Surface Details 115 µm tool 115 µm molded part 10 µm 50 µm P115

13 Effect of Mold Temperature and Cure Time s 25 s 40 s s 25 s 40 s Height Ratio µm tool Mold Temperature ( C) Diameter Ratio µm tool Mold Temperature ( C) No effect on feature diameter and height

14 With High Temperature and Time 50-µm molded part 200 µm 50-µm tool after molding 50 µm P50 with T mold = 210 C Adhesion of LSR in mold cavities stretching and rupture of features

15 Effect of Shot Size 93% 96% 99% 100 µm 100 µm 100 µm Shot Size 93 % 96 % 99 % Diameter Ratio, % 99 ± ± 0 99 ± 0 Height Ratio, % 107 ± ± ± 1 T mold = 160 C; t cure = 10 s Feature replication unaffected by shot size

16 Effect of Switchover Method Switchover Method Position Pressure Diameter Ratio, % 100 ± ± 0 Height Ratio, % 101 ± 0 96 ± 2 Position Pressure 100 µm 100 µm T mold = 160 C; t cure = 10 s Replication unaffected by switchover method

17 Effect of Vacuum Venting 50 µm 10 µm Vacuum Vacuum No Vacuum Vacuum No Vacuum Diameter Ratio, % 101 ± ± ± 1 95 ± 2 Height Ratio, % 102 ± ± ± ± 2 50 µm 10 µm 50 µm 50 µm 10 µm 10 µm V NV V NV T mold = 160 C; t cure = 10 s Feature replication not affect by vacuum venting

18 2: Nanostructured Surfaces Tooling Diameter (Width), Resultant µm Aspect Ratio Spacing Ratio P P P T T Anti-stiction coating: perfluorooctyl-trichlorosilane

19 Processing Conditions Study 1 Study 5 T melt, C ~20 C - due to water cooled barrel T mold, C 160, 185, t cure, s 10, 25, Post Cure 4 h at 200 C Inj. Rate, mm/s 25 x 10-3 mm 3 /s Holding 14 MPa for 30 s 14 MPa for 15 s Vacuum Yes Yes Shot Size, % Switchover Method Position Position Tooling All All < 1 um

20 Results for Nanostructured Surfaces 0.96 µm 0.35 µm 1 µm 0.25 µm 0.95 µm 0.35 µm Feature replication depended on 1) feature size and shape and 2) molding conditions

21 Effect of Mold Temperature T mold = 160 C T mold = 185 C T mold = 210 C T0.95 AR ~ 1.06 P0.96 AR ~ 0.74 Curing time = 10 s Higher mold temperatures 1) Collapse of 0.95-um-wide walls 2) Complete rupture of 0.96-um pillars

22 Effect of Curing Time t cure = 10 s (40 s) t cure = 25 s (55 s) t cure = 40 s (70 s) T0.95 P0.96 Mold temperature = 160 C At longest cure times, tearing of pillars and deformation (wrinkling) of land

23 Effect of Curing Time t cure = 10 s (40 s) t cure = 25 s (55 s) t cure = 40 s (70 s) 1 µm 1 µm 1 µm P µm 1 µm 1 µm P µm 1 µm T0.35 Mold temperature = 160 C

24 Complications from Hold Time t cure = 10 s (25 s) Shorter hold time shorter total curing time Hold time depends on gate size and gate design With higher mold temperatures Total cure time too long for good feature replication t cure = 10 (40 s) Gate design trade off between 1) uniform flow of LSR into features and 2) required hold time T mold = 210 C, t cure = 10 s, t hold = 15 s and 30 s T0.95

25 Effect of Feature Size and Shape on HR Height ratio Was independent of cure time Increased with feature size and crosssection Tooling Height Ratio P ± 0.10 P ± 0.02 P ± 0.03 T ± 0.02 T ±?? Height Ratio µm pillars 0.95 µm trenches 0.35 µm pillars 0.35 µm trenches 0.25 µm pillars PDMS Curing Time (s) Mold temperature = 160 C

26 Effect of Feature Size and Shape on DR Diameter ratio Increased for smaller features Due to greater expansion of curing LSR Tooling Diameter Ratio P ± 0.01 P ± 0.03 P ± 0.09 T ± 0.01 T ± 0.05 Diameter Ratio µm pillars 0.95 µm trenches µm pillars 0.35 µm trenches 0.25 µm pillars PDMS Curing Time (s) Mold temperature = 160 C

27 Comparison of LSR and PDMS LSR and PDMS had similar height ratios LSR had greater diameter ratios LSR features had fewer defects T0.35 PDMS LSR 10 µm 10 µm T0.95 DR = 1.02 ± 0.03 HR = 0.90 ± 0.01 DR = 1.12 ± 0.01 HR = 0.87 ± 0.02

28 Conclusions Complete replication of microfeatures in LSR Independent of curing temperature and time Not affected by shot size, switchover method, and vacuum venting Tearing of features at higher temperatures Replication of LSR nanofeatures Required lower curing temperatures and times to prevent tearing of features Depended on feature size and shape Provided better surfaces than PDMS Can be replicated, but more sensitive to gate size and design Marisely De Jesus Vega and Carol Forance Barry University of Massachusetts Lowell

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