No / This study investigates the influence of length scale effects (micro- and macro-injection molded parts) and mold temperature on the epitaxial growth and morphological characteristics in injection-molded bars of isotactic polypropylene (iPP)/high-density polyethylene (HDPE) blends. After preparing the blends with an iPP content of 70 wt% via melt extrusion, the injection-molded bars were formed using both micro and conventional injection molding. Samples were subsequently prepared from the moulded components to allow investigation of the internal morphology using wide-angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and polarized light microscopy (PLM). The results indicated that the matching of micro scale and appropriate mold temperature was most favorable for epitaxial crystallization. The micro-parts had a large fraction of shear layer compared with macro-parts. The SEM observations showed that the shear layer of the former consisted of a highly oriented shish-kebab structure. Moreover, the effects of different methods of injection molding on the morphological characteristics of the micro-parts and macro-parts in different layers were elucidated in detail using PLM and SEM.

Yes / Micro-injection moulding (μIM) stands out as preferable technology to enable the mass production of polymeric components with micro- and nano-structured surfaces. One of the major challenges of these processes is related to the quality assurance of the manufactured surfaces: the time needed to perform accurate 3D surface acquisitions is typically much longer than a single moulding cycle, thus making impossible to integrate in-line measurements in the process chain. In this work, the authors proposed a novel solution to this problem by defining a process monitoring strategy aiming at linking sensitive in-line monitored process variables with the replication quality. A nano-structured surface for antibacterial applications was manufactured on a metal insert by laser structuring and replicated using two different polymers, polyoxymethylene (POM) and polycarbonate (PC). The replication accuracy was determined using a laser scanning confocal microscope and its dependence on the variation of the main μIM parameters was studied using a Design of Experiments (DoE) experimental approach. During each process cycle, the temperature distribution of the polymer inside the cavity was measured using a high-speed infrared camera by means of a sapphire window mounted in the movable plate of the mould. The temperature measurements showed a high level of correlation with the replication performance of the μIM process, thus providing a fast and effective way to control the quality of the moulded surfaces in-line. / MICROMAN project (“Process Fingerprint for Zero-defect Net-shape MICRO MANufacturing”, http://www.microman.mek.dtu.dk/) - H2020 (Project ID: 674801), H2020 agreement No. 766871 (HIMALAIA), H2020 ITN Laser4Fun (agreement No. 675063)

Yes / Inspired from the low wetting properties of Lotus leaves, the fabrication of dual micro/nano-scale topographies is of interest to many applications. In this research, superhydrophobic surfaces are fabricated by a process chain combining ultrashort pulsed laser texturing of steel inserts and injection moulding to produce textured polypropylene parts. This manufacturing route is very promising and could be economically viable for mass production of polymeric parts with superhydrophobic properties. However, surface damages, such as wear and abrasion phenomena, can be detrimental to the attractive wetting properties of replicated textured surfaces. Therefore, the final product lifespan is investigated by employing mechanical cleaning of textured polypropylene surfaces with multipurpose cloths following the ASTM D3450 standard. Secondly, the surface damage of replication masters after 350 injection moulding cycles with glass-fiber reinforced polypropylene, especially to intensify mould wear, was investigated. In both cases, the degradation of the dual-scale surface textures had a clear impact on surface topography of the replicas and thus on their wetting properties, too. / Europe Union H2020 research and innovation programme.

This thesis investigates the use of micro-injection moulding (μIM), as a high-volume process, for producing three-dimensional, integrated microfluidic devices. It started with literature reviews that covered three topics: μIM of thermoplastic microfluidics, designing for three-dimensional (3-D) microfluidics and functional integration in μIM. Research gaps were identified: Designing 3-D microfluidics within the limitations of μIM, process optimisation and the integration of functional elements. A process chain was presented to fabricate a three-dimensional microfluidic device for medical application by μIM. The thesis also investigated the effect of processing conditions on the quality of the replicated component. The design-of-experiments (DOE) approach is used to highlight the significant processing conditions that affect the part mass taking into consideration the change in part geometry. The approach was also used to evaluate the variability within the process and its effect on the replicability of the process. Part flatness was also evaluated with respect to post-filling process parameters. The thesis investigated the possibility of integrating functional elements within μIM to produce microfluidic devices with hybrid structures. The literature reviews highlighted the importance of quality control in high-volume micromoulding and in-line functional integration in microfluidics. A taxonomy of process integration was also developed based on transformation functions. The experimental results showed that μIM can be used to fabricate microfluidic devices that have true three-dimensional structures by subsequent lamination. The DOE results showed a significant effect of individual process variables on the filling quality of the produced components and their flatness. The geometry of the replicated component was shown to have effect on influential parameters. Other variables, on the other hand, were shown to have a possible effect on process variability. Optimization statistical tools were used to improve multiple quality criteria. Thermoplastic elastomers (TPE) were processed with μIM to produce hybrid structures with functional elements.

Yes / Industry-standard quality management systems such as Six Sigma and emerging Industry 4.0 compliant production processes demonstrate the importance of in-line condition monitoring of manufacturing methods for achieving the highest levels of product quality. Measurement data collected as the process is running can inform the operator about unexpected changes in machine operation or raw materials that could negatively impact production; and offer an opportunity for a process control intervention to stabilise production. However, micro-manufacturing production lines can pose a challenging environment for deploying such systems, since processing events can occur extremely rapidly and in harsh environments. Moreover, the small scale of micro-nano featured components can make sensor installation even more problematic. Recently, ultrasonic micromoulding has drawn attention in niche markets due to its unique advantages for processing thermoplastics as a new micro-manufacturing technology. The process differs from conventional moulding significantly by eliminating the need for a plasticising screw and using direct application of ultrasonic energy to melt the polymer. This offers numerous benefits such as decrease in energy usage, moulding at lower pressures, easier cleaning, and reduced material residence times, the latter which could be beneficial for pharma-grade polymers or polymers with active ingredients. However, very little work has been reported attempting to monitor the process using in-line measurements. This work aims to evaluate the characteristics of the ultrasonic micromoulding process for microinjection moulding of a microneedle array using a range of sensor technologies including: data recorded by the machine controller; a high-speed thermal camera and a cavity pressure transducer. The data has captured the highly dynamic process environment with a high degree of accuracy. The relationship between the process data and dimensional quality of the ultrasonically micromoulded products has been quantified and subsequently implemented as a cost-effective in-line quality assurance method. / Horizon 2020, the EU Framework Programme for Research and Innovation (Project ID: 674801). This research has also received funding and support from two other Horizon 2020 projects: HIMALAIA (Grant agreement No. 766871) and Laser4Fun (GA no. 675063)

Yes / Ultrasound injection molding has emerged as an alternative production route for the manufacturing of micro-scale polymeric components, where it offers significant benefits over the conventional micro-injection molding process. In this work, the effects of ultrasound melting on the mechanical and morphological properties of micro-polypropylene parts were characterized. The ultrasound injection molding process was experimentally compared to the conventional micro-injection molding process using a novel mold, which allows mounting on both machines and visualization of the melt flow for both molding processes. Direct measurements of the flow front speed and temperature distributions were performed using both conventional and thermal high-speed imaging techniques. The manufacturing of micro-tensile specimens allowed the comparison of the mechanical properties of the parts obtained with the different processes. The results indicated that the ultrasound injection molding process could be an efficient alternative to the conventional process.

Yes / Plasma technology has been widely used to increase the surface energy of the polymer surfaces for many industrial applications; in particular to increase in wettability. The present work was carried out to investigate how surface modification using plasma treatment modifies the surface energy of micro-injection moulded microneedles and its influence on drug delivery. Microneedles of polyether ether ketone and polycarbonate and have been manufactured using micro-injection moulding and samples from each production batch have been subsequently subjected to a range of plasma treatment. These samples were coated with bovine serum albumin to study the protein adsorption on these treated polymer surfaces. Sample surfaces structures, before and after treatment, were studied using atomic force microscope and surface energies have been obtained using contact angle measurement and calculated using the Owens-Wendt theory. Adsorption performance of bovine serum albumin and release kinetics for each sample set was assessed using a Franz diffusion cell. Results indicate that plasma treatment significantly increases the surface energy and roughness of the microneedles resulting in better adsorption and release of BSA.

The emergence of microneedle (MN) technologies offers a route for a pain free, straightforward and efficient way of transdermal drug delivery, but technological barriers still exist which pose significant challenges for manufacture of MN systems with high volume outputs at low cost. The main aim of this research was to develop new ways for MN manufacture primarily using micro-injection moulding processes with high performance engineering thermoplastics. During the moulding process these polymeric melts will be subjected to extreme stress and temperature gradients and detailed material characterisation combined with in-line monitoring is desirable to optimise the moulding parameters and will help in achieving sharp microneedles with acceptable quality. Hence high shear rheology of these selected materials was performed at wall shear rates carried out in excess of 107 s-1 over a range of temperatures to predict the flow behaviour of polymer melts at such high shear strain rates. This information was fed into injection moulding simulation software tools (Moldflow) to assist the MN production process design. The optimal design was then used to produce a full 3D solid model of the injection mould and mould insert. Furthermore various design of experiments were conducted considering input parameters such as injection pressure, injection speed, melt temperature, filling time and mould cavity temperature. Response variables including product quality and data acquired from the cavity pressure and temperature transducers were used to optimise the manufacturing process. The moulded MNs were geometrically assessed using a range of characterisation techniques such as atomic force microscopy, confocal microscopy and scanning electron microscopy. An attempt to make hollow MNs was performed and encountered many challenges like partial cavity filling and part ejection during processing. Studies were carried out to understand the problem and identified the major problem was in tool design and improvements to the moulding tool design were recommended. Plasma treatment and mechanical abrasion were employed to increase the surface energy of the moulded polymer surfaces with the aim of enhancing protein adsorption. Sample surface structures before and after treatment were studied using AFM and surface energies have been obtained using contact angle measurement and calculated using Owens-Wendt theory. Adsorption performance of bovine serum albumin and release kinetics for each sample set was assessed using a Franz diffusion cell. Results indicate that plasma treatment significantly increases the surface energy and roughness resulting in better adsorption and release of BSA. To assist design-optimisation and to assess performance, a greater understanding of MN penetration behaviour is required. Contact stiffness, failure strength and creep behaviour were measured during compression tests of MN against a steel surface, and in-vitro penetration of MNs into porcine skin. The MN penetration process into porcine skin was imaged using optical coherence tomography. Finally, a finite element model of skin was established to understand the effect of tip geometry on penetration. The output of findings from this research will provide proof of concept level development and understanding of mechanisms of MN penetration and failure, facilitating design improvements for micro-injection moulded polymeric MNs.

This thesis focuses on the use of a design of experiment approach to examine the significance of process factors and interactions on the fabrication of micro- textured surfaces. The micro-textured surfaces examined contain pillar and hole features ranging from 80 – 2 micrometers in diameter. The processes examined are the deep reactive ion etching of silicon wafers for the production of silicon mould inserts and the micro-injection moulding of polypropylene, high density polyethylene and 316LS stainless steel replicate samples of the silicon mould insert. During the deep reactive ion etching of the silicon wafers the design of experiment approach was used to determine the significant of platen power, C4F8 gas flow and switching times to the presence of pillar undercut of 10 x 10, 5 x 5 and 2 x 2 micrometer pillars. Undercuts occur when the pillar base has a smaller cross-section than the apex of the pillar. Switching times was found to be the only statistically significant parameter for both 10 x 10 and 5 x 5 micrometer pillars. The design of experiment approach is used in the micro-injection moulding of polypropylene, high density polyethylene and 316LS stainless steel replicates to examine the significance of mould temperature, cooling time, holding pressure and injection speed on the part and buffer mass of the produce samples, the height and width of pillar on the replicate surfaces and the variation of the replicated pillars height and width from the original silicon mould insert. Examination of the high density polyethylene replicates found that mould temperature was the most significant factor regarding pillar dimensions (and variation from the silicon mould insert) across the range of pillar sizes. Upon examination of the polypropylene replicates it was found that the factor of most significance on pillar dimensions varied across the different pillar sizes. Holding pressure was identified as the most significant factor with regards to the 53 x 29 and 19 x 80 micrometer pillars. Injection speed was found to be most significant for the 25 x 25 and 19 x 29 micrometer pillars. Cooling time was found to be most significant with regards to the 30 x 10, 25 x 10, 20 x 10 and 15 x 10 micrometer pillars. While ii mould temperature was found to be most significant for the 20 x 20, 15 x 15 and 10 x 30 micrometer pillars. The interaction between mould temperature and injection speed was also found to be the most significant factor with regards to the 43 x 29 and 25 x 30 micrometer pillars. Examination of the 316LS replicates found that mould temperature was the most significant factor regarding pillar dimensions for 80 x 80 and 19 x 80 micrometer pillars. While holding pressure was found to be most significant to the 29 x 29 micrometer pillars and injection speed was identified as most significant to the 53 x 80 micrometer pillars. The samples produced during the design of experiment investigations were then used to examine the effect of surface texturing on droplet behaviour. Droplet contact angles were examined on polypropylene, high density polyethylene and silicon samples structured with 10 – 2 micrometer pillar. Initial droplet contact angles were found to be higher on the polypropylene samples than the high density polyethylene or silicon samples. With the lowest initial contact angles being found for the silicon inserts. Droplet ‘channelling’ and evaporation were examined on silicon, polypropylene, high density polyethylene and 316LS samples structured with micro-channel surface pillars and holes ranging from 80 – 2 micrometer in diameter. Contact pinning of the droplet to the surface via the three- phase contact-line was noted during observations of droplet ‘channelling’. This pinning effect was observed at all sample tilt angles (30 - 90 o ). With regards to droplet evaporation, the droplets were noted to evaporate evenly (with no or limited contact pinning) on all unstructured surfaces and the surfaces structured with hole features. On the surfaces structured with pillar features, the droplets appeared too evaporated along the surface gradient from the smallest pillars to the largest.

The emergence of microneedle (MN) technologies offers a route for a pain free, straightforward and efficient way of transdermal drug delivery, but technological barriers still exist which pose significant challenges for manufacture of MN systems with high volume outputs at low cost. The main aim of this research was to develop new ways for MN manufacture primarily using micro-injection moulding processes with high performance engineering thermoplastics. During the moulding process these polymeric melts will be subjected to extreme stress and temperature gradients and detailed material characterisation combined with in-line monitoring is desirable to optimise the moulding parameters and will help in achieving sharp microneedles with acceptable quality. Hence high shear rheology of these selected materials was performed at wall shear rates carried out in excess of 107 s-1 over a range of temperatures to predict the flow behaviour of polymer melts at such high shear strain rates. This information was fed into injection moulding simulation software tools (Moldflow) to assist the MN production process design. The optimal design was then used to produce a full 3D solid model of the injection mould and mould insert. Furthermore various design of experiments were conducted considering input parameters such as injection pressure, injection speed, melt temperature, filling time and mould cavity temperature. Response variables including product quality and data acquired from the cavity pressure and temperature transducers were used to optimise the manufacturing process. The moulded MNs were geometrically assessed using a range of characterisation techniques such as atomic force microscopy, confocal microscopy and scanning electron microscopy. An attempt to make hollow MNs was performed and encountered many challenges like partial cavity filling and part ejection during processing. Studies were carried out to understand the problem and identified the major problem was in tool design and improvements to the moulding tool design were recommended. Plasma treatment and mechanical abrasion were employed to increase the surface energy of the moulded polymer surfaces with the aim of enhancing protein adsorption. Sample surface structures before and after treatment were studied using AFM and surface energies have been obtained using contact angle measurement and calculated using Owens-Wendt theory. Adsorption performance of bovine serum albumin and release kinetics for each sample set was assessed using a Franz diffusion cell. Results indicate that plasma treatment significantly increases the surface energy and roughness resulting in better adsorption and release of BSA. To assist design-optimisation and to assess performance, a greater understanding of MN penetration behaviour is required. Contact stiffness, failure strength and creep behaviour were measured during compression tests of MN against a steel surface, and in-vitro penetration of MNs into porcine skin. The MN penetration process into porcine skin was imaged using optical coherence tomography. Finally, a finite element model of skin was established to understand the effect of tip geometry on penetration. The output of findings from this research will provide proof of concept level development and understanding of mechanisms of MN penetration and failure, facilitating design improvements for micro-injection moulded polymeric MNs.