Morphology analysis of PEEK 450G using scanning electron microscopy directly on fast scanning calorimetry chips.

To explore the morphology of polyetheretherketone (PEEK), this study employed fast scanning calorimetry (FSC) and scanning electron microscopy (SEM). The objective was to observe the PEEK microstructure under various thermal profiles replicating the additive manufacturing material extrusion process. Samples were observed using SEM directly from the FSC chips, allowing high-accuracy evaluation of the microstructure relative to the thermal profiles. This approach allowed for the evaluation of the microstructure with high accuracy concerning the thermal profiles to which the samples were previously exposed. Each sample was coated with a 10 nm layer of gold-palladium (20-80% ratio), and no etching was necessary to observe the micro features of the microstructure. The approach enabled successful observation and quantification of PEEK microstructure, linking substrate temperature and temperature peaks to microstructural outcomes. Notably, temperature peaks during the process enhanced the formation of well-developed, thick lamellae due to increased chain mobility. Additionally, embryos formed post-remelting of the substrate structure were observed.

Multiscale Porous Poly (Ether-Ether-Ketone) Structures Manufactured by Powder Bed Fusion Process.

The aim of the study is to create a multiscale highly porous poly (ether-ether-ketone) (PEEK) structure while maintaining mechanical performance; the distribution of pores being generated by the manufacturing process combined with a porogen leaching operation. Salt at 70 wt% concentration was used as a porogen in a dry blend with PEEK powder sintered in the powder bed fusion process. The printed porous PEEK structures were examined and evaluated by scanning electron microscopy, microcomputed tomography, and mechanical testing. The PEEK structures incorporating 70 wt% salt achieved 79-86% porosity, a compressive yield strength of 4.1 MPa, and a yield strain of ∼60%. Due to the salt leaching process, the PEEK porous frameworks were fabricated without the need to drastically reduce the process parameters (defined by the energy density [ED]), hence maintaining the structural integrity and good mechanical performance. The compression results highlighted that the performance is influenced by the printing orientation, level of the PEEK particle coalescence (controlled here by the ED), pore/cell wall thickness, and subsequently, the overall porosity framework. The porous printed PEEK structures could find potential uses in a wide range of applications from tissue engineering, filtration and separation to catalysts, drug release, and gas storage.

Adaptable polyaryletherketones (PAEKs) with competing crosslinking and crystallisation mechanisms.

Driven by the need to make high temperature thermoplastic polymers more processable and expand the range of applications, this study reports on the properties of a novel PAEK material developed by Victrex (Thornton Cleveleys, UK) which is capable of undergoing crosslinking or crystallisation, two competing processes that can be adapted via specific processing temperature and time conditions. The uniqueness of this PAEK material resides in its manufacturing approach, where the crosslinkers are incorporated during the polymerisation process, and its distinct properties, including a controllable viscosity that can be tuned from low to high to allow its application in complex manufacturing processes, such as thermoplastic carbon fibre manufacturing.

Prototype Design for Grading Structures in Powder Bed Fusion Processes.

While targeted alignment in certain additive manufacturing (AM) methods such as material extrusion (MEX) and stereolithography (SLA) has been well documented in the research community, a method for targeted alignment of added fillers or fibrous materials in powder bed fusion (PBF) AM devices has yet to be successfully achieved. Similarly, incorporation of multimaterials does not work easily with any of the AM technologies. This study creates a prototype design that could be integrated into a PBF system to allow for multimaterial layer deposition and alignment of powders and powder blends. The rheological properties of polyamide powder and a range of polyamide composite blends (incorporating milled carbon fibre, graphite flakes, polytetrafluoroethylene, and glass microspheres) in different concentrations were studied, and together with the particle size distribution and particle morphology analysis were applied for the design of a prototype hopper for incorporation in the PBF system to create targeted multimaterial deposition. Different concept designs, multichambered and multi-hopper with hopper angles calculated specifically for the composite blend powders selected, were proposed. Initial deposition trials outside a PBF process were tested, and the deposited layers were measured.

Powder Bed Fusion Versus Material Extrusion: A Comparative Case Study on Polyether-Ether-Ketone Cranial Implants.

As the choice of additive manufacturing (AM) technologies is becoming wider with reliable processes and a wider range of materials, the selection of the right technology to fabricate a certain product is becoming increasingly difficult from a technical and cost perspective. In this study polyether-ether-ketone cranial implants were manufactured by two AM techniques: powder bed fusion (PBF) and fused filament fabrication (FFF) and their dimensional accuracy, compression performance, and drop tower impact behavior were evaluated and compared. The results showed that both types of specimens differed from the original computer-aided design; although the origin of the deviation was different, the PBF samples were slightly inaccurate owing to the printing process where the accuracy of the FFF samples was influenced by postprocessing and removal of the scaffolds. The cranial implants fabricated using the FFF method absorbed more energy during the compression and impact tests in comparison with the PBF process. The failure mechanisms revealed that FFF samples have a higher ability to deform and a more consistent failure mechanisms, with the damage localized around the puncture head region. The brittle nature of the PBF samples, a feature observed with other polymers as well, led to complete failure of the cranial implants into several pieces.

Enhanced Ductility of PEEK thin film with self-assembled fibre-like crystals.

Poly Ether Ether Ketone (PEEK) is a high temperature polymer material known for its excellent chemical resistance, high strength and toughness. As a semi-crystalline polymer, PEEK can become very brittle during long crystallisation times and temperatures helped as well by its high content of rigid benzene rings within its chemical structure. This paper presents a simple quench crystallization method for preparation of PEEK thin films with the formation of a novel fibre-like crystal structure on the surface of the films. These quenched crystallised films show higher elongation at break when compared with conventional melt crystallised thin films incorporating spherulitic crystals, while the tensile strength of both types of films (quenched crystallised and conventional melt) remained the same. The fracture analysis carried out using microscopy revealed an interesting microstructure which evolves as a function of annealing time. Based on these results, a crystal growth mechanism describing the development of the fibre-like crystals on the surface of the quenched crystallised films is proposed.

Quantitative analysis of the distribution and mixing of cellulose nanocrystals in thermoplastic composites using Raman chemical imaging.

Cellulose nanofibers hold much promise for enhancing the mechanical properties of composites owing to their uniquely high stiffness and strength. One major issue limiting this performance however is the dispersion and mixing of cellulose nanofibers within thermoplastic resins. A combination of Raman imaging and chemical analysis has been used to quantify the distribution and mixing of cellulose nanocrystals (CNCs) in a polyethylene-matrix composite. Large area spectral imaging provides information about the effect of a compatibilizer - namely poly(ethylene oxide) (PEO) and maleated polyethylene (MAPE) - on the distribution of CNCs in the thermoplastic matrix. High-resolution images enable quantification of the degree of mixing between the CNCs and HDPE. Lower resolution images, but with greater spatial spread, allow quantification of the distribution of the CNCs. It is shown that the CNCs tend to agglomerate, with little increase in distribution even with the use of the compatibilizer. A shift in the position of characteristic Raman bands indicates the formation of hydrogen bonding between the PEO compatibilizer and the CNCs, which in turn is thought to affect the distribution of aggregates of the reinforcing phase.

Poly Aryl Ether Ketones (PAEKs) and carbon-reinforced PAEK powders for laser sintering.

This paper discusses various methods of fabrication of plain and carbon-reinforced composite powders, as well as a range of powder characterisation test methods suitable for defining powders for laser sintering. Two milling processes (based on disc blades and rotatory cutting knives) were used as methods of fabrication of powders, starting from injection moulding granule grades, for comparison with current powders obtained directly from polymerisation processes. It was found that the milling process affects the particles properties. The rotary milling produced powders with superior properties in comparison with the disc milling method. Tests including particle size distribution, angle of repose, aspect ratio, sphericity and roundness of particles were employed to compare and assess the suitability of powders for laser sintering. The Brunauer-Emmett-Teller test was identified as a useful method to define surface roughness and porosity of the particles. The carbon fibre (Cf) Poly Ether Ketone (PEK) granules milled well and after an additional sieving process created a good quality powder. This is the first attempt to investigate properties of PEK powder with encapsulated Cf and follow their sintering profile through hot-stage microscopy. It is expected that this type of composite powder will create isotropic structures in comparison with the highly anisotropic properties given by the known dry mix composite powders, currently used in laser sintering.

High yield growth of patterned vertically aligned carbon nanotubes using inkjet-printed catalyst.

This study reports on the fabrication of vertically aligned carbon nanotubes localized at specific sites on a growth substrate by deposition of a nanoparticle suspension using inkjet printing. Carbon nanotubes were grown with high yield as vertically aligned forests to a length of approximately 400 µm. The use of inkjet printing for catalyst fabrication considerably improves the production rate of vertically aligned patterned nanotube forests compared with conventional patterning techniques, for example, electron beam lithography or photolithography.

Monomer conversion and hardness of novel dental cements based on ethyl cyanoacrylate.

OBJECTIVES: The aim of this work was to study the setting of two novel dental cements: (i) a 'hybrid' cement, incorporating an ethyl cyanoacrylate into a glass-ionomer cement (ECGIC) formulation and (ii) an ethyl cyanoacrylate/hydroxyapatite composite cement (ECHC). The mechanical role of the cyanoacrylate and its curing within the cements have been discussed. METHODS: The setting of the cements was characterised using Vickers indentation hardness and near-infrared (near-IR) spectroscopy. RESULTS: The cyanoacrylate component of ECGIC was 100% cured approximately 10min after the initial cement mixing. The ECGIC continued to increase in hardness after the cyanoacrylate component was fully cured. This proved that the fully polymerised network of cyanoacrylate did not prevent the acid-base reactions of the GIC components from continuing. The Vickers hardness number of ECGIC at 18 weeks was approximately 105. The curing of the cyanoacrylate within ECHC was much slower and was still not complete (98%) 18 weeks after the initial cement mixing. The hardness of the ECHC was shown to be correlated with the extent of cyanoacrylate cure. The Vickers hardness number of ECHC at 18 weeks was approximately 21. The primary reasons for the overall lower hardness of ECHC in comparison to ECGIC were the lower powder:liquid ratio and the softer filler type. SIGNIFICANCE: Careful consideration is needed when incorporating cyanoacrylates into dental cements, as speed of cure and hardness are particularly important.