The manufacture of polyetheretherketone/hydroxyapatite (PEEK/HA) composites is seen as a viable approach to help enhance direct bone apposition in orthopaedic implants. A range of methods have been used to produce composites, including Selective Laser Sintering and injection moulding. Such techniques have drawbacks and lack flexibility to manufacture complex, custom-designed implants. 3D printing gets around many of the restraints and provides new opportunities for innovative solutions that are structurally suited to meet the needs of the patient. This work reports the direct 3D printing of extruded PEEK/HA composite filaments via a Fused Filament Fabrication (FFF) approach. In this work samples are 3D printed by a custom modified commercial printer Ultimaker 2+ (UM2+). SEM-EDX and µCT analyses show that HA particles are evenly distributed throughout the bulk and across the surface of the native 3D printed samples, with XRD highlighting up to 50% crystallinity and crystalline domains clearly observed in SEM and HR-TEM analyses. This highlights the favourable temperature conditions during 3D printing. The yield stress and ultimate tensile strength obtained for all the samples are comparable to human femoral cortical bone. The results show how FFF 3D printing of PEEK/HA composites up to 30 wt% HA can be achieved.

The present review provides an overview of the current status and future perspectives of one of the smart manufacturing techniques of Industry 4.0, laser transmission welding (LTW) of semi-crystalline (SC) polymers and their composites. It is one of the most versatile techniques used to join polymeric components with varying thickness and configuration using a laser source. This article focuses on various parameters and phenomena such as inter-diffusion and microstructural changes that occur due to the laser interaction with SC polymers (specifically polypropylene). The effect of carbon black (size, shape, structure, thermal conductivity, dispersion, distribution, etc.) in the laser absorptive part and nucleating agent in the laser transmissive part and its processing conditions impacting the weld strength is discussed in detail. Among the laser parameters, laser power, scanning speed and clamping pressure are considered to be the most critical. This review also highlights innovative ideas such as incorporating metal as an absorber in the laser absorptive part, hybrid carbon black, dual clamping device, and an increasing number of scans and patterns. Finally, there is presented an overview of the essential characterisation techniques that help to determine the weld quality. This review demonstrates that LTW has excellent potential in polymer joining applications and the challenges including the cost-effectiveness, innovative ideas to provide state-of-the-art design and fabrication of complex products in a wide range of applications. This work will be of keen interest to other researchers and practitioners who are involved in the welding of polymers.

Hardness is a useful measure of a material’s resistance to permanent indentation; but for viscoelastic polymers, hardness data are highly dependent on the test type and the parameter set chosen. Vickers microhardness testing is used to leave small indents (<150 µm) and is shown to be applicable to polymers. A detailed investigation of the required steps for microhardness testing in isotactic polypropylene (iPP) is provided. Samples should be mounted in epoxy resin in order to maintain curing temperatures at room temperature. Mounted samples can be ground and polished in a semi-automatic polisher using graduated SiC paper (wet grinding) but progressing onto alumina suspension for polishing. Final polishing should be performed with 0.05-µm alumina suspension. The hardness measured was shown to be dependent on load and dwell time with a much greater dependency on dwell time. Strain recovery was shown to be completed after a time period equal to the dwell time. This study shows that indents can be measured thereafter, and it is recommended that they be measured within a 24 h period after the indent was created. After data fitting, the equation for hardness was shown to follow a power law with load and dwell time as the main variables. Fitting parameters were compared to those found in the literature, and it was found that parameters were significantly different to those reported elsewhere. Therefore, this study highlights the importance of calibrating on a case-by-case basis. Finally, to show the usefulness of the Vickers micro-hardness testing method, the calibrated test method was applied on iPP with additions of carbon black up to 3 wt.%. Comparisons were made with data from the literature, but the hardness data generated in our work were found to be at least twice that reported in the literature. The testing parameters were not cited in the literature: specifically, the dwell time was not provided, and this generated doubt on the usefulness of the cited data. Hence, this work is intended to serve as an exemplar of how to prepare and proceed with hardness testing of polymers.

Laser welding is an important manufacturing tool for a wide variety of polymer products including consumer goods, automotive components and medical devices. The laser process parameters and polymer properties have a significant impact on weld quality. Due to higher heat density generated by the laser transmission welding (LTW) technique, defining a set of suitable parameters for LTW of thermoplastics and composites can be challenging. In this work the effect of carbon black along other control parameters has been investigated for high speed welding using a laser source of 980 nm wavelength with low line energy. In this work, the finite element method (FEM)-based software COMSOL Multiphysics is used to create a 3D transient thermal model for LTW of isotactic polypropylene (iPP) and its composites with carbon black (CB) of concentrations ranging from 0.5 wt% to 1.5 wt%. The design of experiments based on Box-Behnken design (BBD) is used to organize the simulation experiments and mathematical models are developed based on multiple curvilinear regression analysis on the simulation findings. Independent control variables include the laser power, welding speed, beam diameter, and carbon black content in the absorbent polymer. The maximum weld temperature, weld width, and weld depth within the transmissive and absorptive layers are considered as dependent response variables. Furthermore, sensitivity analysis is carried out to investigate the impact of carbon black along with other independent variables on the responses. The welding feasibility check was performed on the basis of melt and degradation temperature of the materials, and weld depths of transmissive and absorptive layers. It has been observed that the composites containing 0.5 wt% and 1 wt% of CB can be welded successfully with neat iPP. However, due to a degradation temperature problem, composites having a larger proportion of CB (&gt;1 wt%) appear to be more difficult to weld.

Variations in mould shrinkage when using organic and inorganic pigments in semicrystalline polymers is a well-known phenomenon within industry. These differences in mould shrinkage are thought to be caused by the presence of the pigments acting as nucleating agents, altering the crystallisation of semicrystalline polymers. These shrinkage variations can give rise to problems in obtaining the correct interference fit between parts and can cause issues in automated equipment such as filling lines. It has been previously reported that the onset temperature of crystallisation measured via DSC (differential scanning calorimetry) can be used to predict shrinkage when a variety of neat pigments are added to un-nucleated PP (polypropylene). However, the shrinkage and crystallisation behaviour of masterbatch pigments, which are widely used industrially is poorly understood. To better understand the influence of masterbatch pigments on crystallisation and shrinkage behaviour, injection moulded samples were prepared using variety of reds, whites, and purple commercial-masterbatch pigments with PP. The crystallisation kinetics and crystallinity were studied using DSC, LPOM (Linkam hot stage polarising optical microscopy), XRD (X-ray diffraction), and FTIR (Fourier transform infrared spectroscopy). The morphology was investigated via LPOM and SEM (scanning electron microscopy). A clear correlation was observed between the crystallisation onset temperature measured using DSC and the recorded shrinkage. A strong relationship was also observed between the percentage crystallinity measured using FTIR and shrinkage. Quinacridone and pyrrole based red and purple pigments were found to act as strong nucleating agents, with the pyrrole based red pigment also acting as β nucleator in PP. The white pigments were found to have less influence on the nucleation behaviour. For the pigments which induced the largest variation in shrinkage, a higher rate of nucleation and proportionally smaller spherulitic diameter was observed by DSC, SEM, and LPOM.