Optimization of printing parameters for improvement of mechanical and thermal performances of 3D printed poly(ether ether ketone) parts

Many processing parameters can be adjusted to optimize the fused filament fabrication (FFF) process, a popular and widely used additive manufacturing techniques for plastic materials. Among those easily adjusted parameters are the nozzle temperature, printing speed, raster orientation, and layer thicknesses. Using poly(ether ether ketone) (PEEK) as the base material, a design of experiments analysis was performed on the main FFF parameters. A response surface methodology was applied to analyze the results and to maximize the output responses. Results have shown that the nozzle temperature is the most influential parameter on tensile properties and the crystallinity degree of printed PEEK by FFF process. Parts produced with optimized FFF parameters were then subjected to an annealing treatment to induce a relaxation of residual stress and to enhance crystallinity. The best properties for 3D printed PEEK parts were achieved with annealed parts prepared at 400°C with a printing speed of 30 mm/s, 0.15 mm layer thickness and raster orientation of [0°/15°/−15°]. The resulting parts have mechanical properties comparable to those of injected PEEK.     

Investigating the effect of printing conditions and annealing on the porosity and tensile behavior of 3D-printed polyetherimide material in Z-direction

Fused filament fabrication process presents drawbacks in mechanical properties observed when printing in the build direction (Z-direction). Such anisotropic properties will affect the part's performances and have to be minimized during fabrication. This study aims to evaluate the effects of nozzle temperature, printing speed and specimen state (annealed or as-printed) on porosity percentage and tensile properties for 3D printed polyetherimide (PEI) (ULTEM 1010) parts in Z-direction. The results demonstrated that print speed is the most influential process parameter that should be adjusted in consideration with the other printing parameters. The specimens' state did not reveal a noticeable influence, as the amorphous nature of PEI is considered less receptive to annealing. The optimization method to achieve the best results yielded values of 360°C and 30 mm s⁻¹ as printing conditions, followed by heat treatment. This was confirmed by porosity measurements, tensile testing, and scanning electron microscopy observations. The best performances of PEI material were 3425.5 MPa, 102 MPa, and 4.30% for Young's modulus, tensile strength, and elongation at break, respectively.     

An Experimental Study of Nozzle Temperature and Heat Treatment (Annealing) Effects on Mechanical Properties of High-Temperature Polylactic Acid in Fused Deposition Modeling

Fused deposition modeling (FDM) is the trendiest three-dimensional (3D) printing method among additive manufacturing technologies. In this process, the final parts are constructed through layer-by-layer adhesion of thermoplastic polymers. Amorphous thermoplastic polymers have better printability compared to semicrystalline ones; so, they are most popular with FDM users. Generally, the overall mechanical properties of FDM 3D printed parts are weaker in comparison to the traditional methods (such as injection molding) due to the weak bonds between the deposited rasters and layers. Therefore, the introduction of new materials with higher mechanical properties and easy printing process of the semicrystalline polymers has always been challenging to progress the mechanical properties of the products. In this study by the FDM process, the effect of nozzle temperature and heat treatment (annealing) on the mechanical properties of high-temperature polylactic acids is investigated. The increase in the nozzle temperature develops the rasters and layers bonding, and the heat treatment of the parts after printing rises the crystallinity percentage, which is crucial for the improvement of mechanical properties. Experimental results show that an increase in the nozzle temperature raises the tensile strength and modulus to 65.7 MPa and 4.97 GPa, respectively. Furthermore, the heat treatment process increases the tensile strength and modulus up to 67.4 MPa and 5.65 GPa. The final tensile modulus values are the highest ones reported for pure materials printed by the FDM process. POLYM. ENG. SCI., 60:979–987, 2020. © 2020 Society of Plastics Engineers     

3D-printed polymer packing structures: Uniformity of morphology and mechanical properties via microprocessing conditions

Three-dimensional (3D) printing is an attractive approach to fabricate highly porous extremely lightweight structures for architecture antivibrational packaging. We report 3D printing processing of model packaging structures using biodegradable poly(lactic acid) (PLA) as a source material, with acrylonitrile butadiene styrene (ABS) utilized as a common 3D printing source material as a traditional benchmarked material. The effects of printing temperature, speed, and layer morphology on the layer-by-layer 3D-printed structures and their mechanical properties were considered. Three different characteristic morphologies were identified based on printing temperature; the microscopic surface roughness was dependent on the printing speed and layer height. We demonstrate that the mechanical performances and surface properties of 3D-printed PLA structures could be improved by optimization of printing conditions. Specifically, we evaluate that these PLA-based 3D structures printed exhibited better surface qualities and enhanced mechanical performance than traditional ABS-based structures. Results showed that the PLA-based 3D structures possessed the favorable mechanical performance with 34% higher Young's modulus and 23% higher tensile strength in comparison to the ABS-based 3D structures. This study provides guidelines for achieving high-quality 3D-printed lightweight structures, including smooth surfaces and durable mechanical properties, and serves as a framework to create biodegradable 3D-printed parts for human use.     

Development of Pure Poly Vinyl Chloride (PVC) with Excellent 3D Printability and Macro- and Micro-Structural Properties

Unmodified polyvinyl chloride (PVC) has low thermal stability and high hardness. Therefore, using plasticizers as well as thermal stabilizers is inevitable, while it causes serious environmental and health issues. In this work, for the first time, pure food-grade PVC with potential biomedical applications is processed and 3D printed. Samples are successfully 3D printed using different printing parameters, including velocity, raster angle, nozzle diameter, and layer thickness, and their mechanical properties are investigated in compression, bending, and tension modes. Scanning electron microscopy is also used to evaluate the bonding and microstructure of the printed layers. Among the mentioned printing parameters, raster angle and printing velocity influence the mechanical properties significantly, whereas the layer thickness and nozzle diameter has a little effect. Images from scanning electron microscopy  also reveal that printing velocity greatly affects the final part's quality regarding defective voids and rasters’ bonding. The maximum tensile strength of 88.55 MPa is achieved, which implies the superiority of 3D-printed PVC mechanical properties compared to other commercial filaments. This study opens an avenue to additively manufacture PVC that is the second most-consumed polymer with cost-effective and high-strength features.     

Parametric optimization of intra‐ and inter‐layer strengths in parts produced by extrusion‐based additive manufacturing of poly(lactic acid)

Parts produced by extrusion‐based additive manufacturing experience the disadvantage of consisting of many weld‐lines, which consequently downgrade their mechanical properties. This work aims at maximizing the strength of printed parts by considering and improving the intra‐ and inter‐layer cohesion between adjacent strands. Therefore, printed poly(lactic acid) specimens were characterized by means of a particular tensile test setup, and the inter‐layer cohesion of printed specimens was evaluated by means of the double cantilever beam test. A detailed parametric statistical evaluation, which included printing temperatures, layer thicknesses, and layer‐designs, was complemented by the material's viscosity data and the analysis of the specimens' fracture surfaces and cross‐sections. An optimal layer‐design was found to be a key parameter in the optimization of strength with regard to different loading directions. Additionally, the maximization of the cohesion leads to a tremendous improvement in the mechanical performance of the printed parts, resulting in strengths of roughly 90% of those of compression‐molded parts. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45401.     

High‐tensile‐strength polyvinyl alcohol films prepared from freeze/thaw cycled gels

The mechanical properties and molecular structure of a poly(vinyl alcohol) (PVA) film, which was obtained by eliminating water from a PVA hydrogel using repeated freeze/thaw cycles, were investigated by tensile tests, thermal analysis, and X‐ray diffraction measurements. The mechanical properties of PVA with 99.9% saponification were measured as a function of the number of freeze/thaw cycles performed. The tensile strength and Young's modulus increased and the elongation at break decreased with increasing freeze/thaw cycles. The tensile strength and Young's modulus of PVA films obtained after seven freeze/thaw cycles were as high as 255 MPa and 13.5 GPa after annealing at 130°C. Thermal analysis and X‐ray diffraction measurements revealed that this is because of a high crystallinity and a large crystallite size. A good relationship between the tensile strength and the glass transition temperature was obtained, regardless of the degree of saponification and annealing conditions. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40578.     

Investigation of 3D printing strategy on the mechanical performance of coextruded continuous carbon fiber reinforced PETG

Fused filament fabrication (FFF) has been used to create prototypes and functional parts for various applications using plastic filaments. It has also been extended to the use of continuous fibers for reinforcing thermoplastic polymers. This study aims to optimize the deposition design of a coextruded continuous carbon fiber (CCF) composite filament with a polyethylene terephthalate glycol-modified (PETG) filament. The characterizations on the raw materials revealed that the matrix polymer in CCF composite filament had similar physicochemical properties as PETG, and carbon fibers were homogeneously distributed in CCF filament. The effect of raster orientation and shells number on the mechanical properties of non-reinforced and coextruded CCF-reinforced PETG was investigated. The highest mechanical properties were obtained at a raster orientation of 0° for both reinforced and non-reinforced materials. With the increase of raster orientation, Young's modulus and ultimate tensile strength decreased. The presence of shells improved the tensile strength of non-reinforced PETG. For composite samples printed with unreinforced shells, Young's modulus decreased due to decrease in fibers content, and elongation at break and ultimate tensile strength increased. Tomographic observations showed that the mechanical behavior of printed specimens depended on the anisotropy of porosity in printed specimens.     

Mechanical and dimensional performance of poly(lactic acid) 3D-printed parts using thin plate spline interpolation

In additive manufacturing, determining the correct deposition parameters is very important as this can affect the final properties of printed parts. Since there is no agreement on the optimal level of the different printing parameters in reported results, this work evaluated the influences of layer thickness (LT), deposition speed (DS) and printing direction (PD) on tensile properties and dimensional accuracy of poly(lactic acid) 3D parts evaluating the possibility of using thin plate spline interpolation method (TPSIM) of data, a new approach, in determination of optimized fused deposition modeling process parameters. It was observed that the use of low levels of LT (0.10 mm), DS (40 mm/s), and PD (0°) provided parts with higher mechanical strength and dimensional performance. Denser parts showed lower anisotropy effect and, consequently, best tensile properties were obtained. TPSIM was an efficient mathematical analysis and well fitted results of predicted and experimental results.     

Quantification of the Young's modulus for polypropylene: Influence of initial crystallinity and service temperature

In this study, the mechanical properties of isotactic polypropylene (iPP) materials with different crystallinities at room and elevated temperatures were investigated. In order to obtain samples with a certain range of crystallinity, and to ensure a uniform microstructure of these samples, the iPP samples obtained by injection molding required melt compression molding and controlled annealing. In the macromechanical studies, the experimental results showed that the storage modulus and Young's modulus of polypropylene were sensitive to the service temperature. The crystallinity also had a great influence on this relationship. A function was proposed to evaluate the dependence of the Young's modulus of polypropylene on initial crystallinity and service temperature, and tested based on experimental data. The Young's modulus of iPP is reduced by about 90% when the service temperature rises from 25 to 125 °C. Moreover, the reduced value in Young's modulus between polypropylene having the highest and lowest crystallinity was reduced from 214.55 to 56.75 MPa. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48581.     

Thermal and mechanical properties of chitosan reinforced polyhydroxybutyrate composites

The article reports the results of studies on the effect of chitosan (0, 5, 10, 20, 30, and 40 wt %) on thermal and mechanical properties of poly(hydroxybutyrate) composites. The addition of chitosan causes an increase in the glass transition temperature (T_g) while a decrease in the enthalpy of fusion (ΔH_fus), crystallization (ΔH_cry) and percentage of crystallinity as determined by differential scanning calorimeter (DSC). The thermogravimetric analysis reveals that high amount of chitosan decreases the thermal stability of the composites. The Young's modulus of the composite increases and is high for the composite having 40 wt % of chitosan. Increase in the amount of chitosan decreases the elongation at break and impact strength of composites. Finally, the Young's modulus of the composites has been compared with the theoretical predictions. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Polyoxymethylene‐homopolymer/hydroxyapatite nanocomposites for biomedical applications

In this article, new polyoxymethylene (POM)/hydroxyapatite (HAp) nanocomposites for bone long‐term implants have been obtained and characterized by using FTIR, WAXD, SEM, TG, DSC, tensile tests, and in vitro evaluation. Characteristic bands both for extended chain crystals (ECC) and folded chain crystals (FCC) were observed in FTIR profiles for both pure POM and POM in POM/HAp nanocomposites. From WAXD analysis it has been found that the addition of HAp does not change the hexagonal system of POM in POM/HAp nanocomposites. Moreover, degree of crystallinity of POM increases with an increase of HAp content up to 1.0% and next decreases with an increase HAp content. It indicates that HAp nanoparticles up to 1.0% content act as effective nucleating sites. Mechanical tests revealed that Young's modulus increases, whereby, elongation at break and tensile strength decrease with increasing hydroxyapatite concentration. Results of in vitro investigations show that an increase of HAp content in POM nanocomposites facilitates formation of apatite layer on the sample surface and improves in vitro stability POM/HAp nanocomposites. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Thermal and mechanical properties of polyamide 12/graphene nanoplatelets nanocomposites and parts fabricated by fused deposition modeling

The printable polyamide 12 (PA12) nanocomposite filaments with 6 wt % graphene nanoplatelets (GNPs) for fused deposition modeling (FDM) were prepared by melting compounding and smoothly printed via a commercial FDM three‐dimensional (3D) printer. The thermal conductivity (λ) and elastic modulus (E) of 3D printed PA12/GNPs parts along to the printing direction had an increase by 51.4% and 7% than that of compression molded parts, which is due to the GNPs preferentially aligning along to the printing direction. Along with these improved properties, ultimate tensile strength of 3D printed PA12/GNPs parts was well maintained. These results indicate that FDM is a new way to achieve PA12/GNPs parts with enhanced λ over compression moulding, which could contribute to realize efficient and flexible heat management for a wide range of applications. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45332.     

Processing–mechanical property relationships in injection moldings of polybutylene

Two unfilled nonpigmented extrusion grades of polybutylene have been injection-molded into a tensile bar mold under a wide range of barrel and mold temperatures. The overall structure of the moldings has been determined and correlated with processing conditions. The short term tensile mechanical properties of the moldings have been ascertained and correlated with molding structure. For low mold temperatures, the Young's modulus and tensile strength of injection moldings of polybutylene are controlled by the extent of and structure within the highly oriented skin. Low barrel temperatures can give rise to highly crystalline thick skins that treble the Young's modulus and fracture stress, when compared to high barrel temperature moldings. Increasing the mold temperature introduces a brittle response in polybutylene injection moldings. Modulus is controlled, at the high mold temperatures, by the skin thickness and by the crystallinity of the material comprising the core of the molding.     

Mechanical Properties of PPS/PC/GF/Nano-CaCO3 Hybrid Composites

A kind of nanometer calcium carbonate (nano-CaCO₃) filled glass fibre-reinforced polyphenylene sulfide/polycarbonate (PPS/PC/GF) hybrid composites were fabricated with a twin-screw extruder in this paper, and the surface of the nanometer particles was pretreated with stearic acid in a high speed mixer before melt blending. The Young's modulus, tensile strength, tensile elongation at break, flexural modulus and strength of these hybrid composites were measured at room temperature by using a universal materials testing machine, to identify the influence of the nano-CaCO₃ content on the mechanical properties of these hybrid composites. It was found that there were relatively evident reinforcing and toughening effects of the nano-CaCO₃ on the PPS/PC/GF hybrid composites. The Young's modulus, tensile strength, flexural strengt and elongation at break of these composites increased nonlinearly with an addition of the nano-CaCO₃ weigh fraction (φ _f ) when φ _f was less than 6%, and they reached the maximum at φ _f of 6%, and then decreased; while the flexural modulus increased as φ _f was less than 4%, and then decreased.     

Effects of laser polishing on surface quality and mechanical properties of PLA parts built by fused deposition modeling

Fused deposition modeling (FDM) produces parts through layer by layer on the top of each other, making it almost impossible to obtain smooth printed parts. Hence, there is a huge demand for the postprocessing of the FDM-printed parts. Laser polishing is a novel technique that can be used to polish products to obtain a smoother surface. The aim of this work was to explore the feasibility of surface-finishing FDM-printed polylactic acid (PLA) parts by laser polishing. The surface roughness, surface morphology, dynamic mechanical analysis (DMA), and tensile properties were investigated. The results indicated that the lower laser power and the bigger laser beam diameter within a certain range could facilitate the formation of smoother surface. With optimized parameters, the surface roughness was reduced by 90.4%. DMA showed that the storage modulus (E’) and glass transition temperature of PLA specimens were significantly improved due to the decrease of molecular mobility of denser structures. Moreover, the tensile strength and Young's modulus of the PLA specimen were also significantly increased after laser polishing. The fracture morphologies were observed, and the possible strengthening mechanism was also discussed. These results indicated that laser polishing could be an efficient method for surface polishing of FDM parts. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48288.     

Phase morphology,thermomechanical, and crystallization behavior of uncompatibilized and PP‐g‐MAH compatibilized polypropylene/polystyrene blends

In this article, we discuss the phase morphology, thermal, mechanical, and crystallization properties of uncompatibilized and compatibilized polypropylene/polystyrene (PP/PS) blends. It is observed that the Young's modulus increases, but other mechanical properties such as tensile strength, flexural strength, elongation at break, and impact strength decrease by blending PS to PP. The tensile strength and Young's modulus of PP/PS blends were compared with various theoretical models. The thermal stability, melting, and crystallization temperatures and percentage crystallinity of semicrystalline PP in the blends were marginally decreased by the addition of amorphous PS. The presence of maleic anhydride‐grafted polypropylene (compatibilizer) increases the phase stability of 90/10 and 80/20 blends by preventing the coalescence. Hence, finer and more uniform droplets of PS dispersed phases are observed. The compatibilizer induced some improvement in impact strength for the blends with PP matrix phase, however fluctuations in modulus, strength and ductility were observed with respect to the uncompatibilized blend. The thermal stability was not much affected by the addition of the compatibilizer for the PP rich blends but shows some decrease in the thermal stability of the blends, where PS forms the matrix. On the other hand, the % crystallinity was increased by the addition of compatibilizer, irrespective of the blend concentration. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42100.     

On the physical behavior of isotactic polypropylene fibers extruded at different draw‐down ratios: II. Structure and properties

Microinterferometry (MIF), wide‐angle X‐ray scattering (WAXS), differential scanning calorimetry (DSC), and an Instron tensile tester (ITT) were used to determine the correlation between optical and structural properties of polypropylene (PP) fibers. For the purpose of the study a set of as‐spun isotactic PP fibers were extruded by melt spinning at different draw‐down ratios (DDR). The birefringence (Δn), degrees of orientation, degree of crystallinity (χ), Young's modulus (E_e), and tenacity (τ) were determined for PP fibers at the different DDR. An equiangular orientation of PP fibers at particular DDR was predicted experimentally, and the transverse modulus (E_t) was estimated for the tested fibers. Empirical formulae were developed for correlating the fiber birefringence with some of the studied structural properties of PP fibers. POLYM. ENG. SCI., 2010. © 2009 Society of Plastics Engineers     

Effect of different film preparation procedures on the thermal,morphological and mechanical properties of pure and calcite‐filled HDPE films

The effect of different film preparation procedures on the thermal, morphological and mechanical properties of high density polyethylene (HDPE) films have been studied using differential scanning calorimetry (DSC), wide angle X‐ray diffraction (WAXRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and ultimate tensile testing. Film preparation procedures included variation in cooling methods, including quenching, forces (fanning) and natural cooling and techniques such as extrusion followed by melt squeezing and compression molding. The heat of fusion (from DSC), the degree of crystallinity (from WAXRD) and the crystallite size (from WAXRD and AFM) were found to be highest for naturally cooled specimens, followed by fan‐cooled and quenched ones. AFM images of surface topology exhibit stacked lamellar morphology for forcefully cooled (fan‐cooled and quenched) samples and spherulitic ‘lozenges’ for naturally cooled ones. The Young's modulus and yield stress [from the universal testing machine (UTM)] were highest for naturally cooled samples, followed by fan‐cooled and quenched ones. Among the calcite‐filled composites, the ‘base film,’ which was prepared by extrusion followed by melt squeezing and natural cooling, exhibited the lowest heat of fusion and degree of crystallinity and a similar crystallite size relative to compression‐molded films. Lower yield stress, tensile strength and Young's modulus and higher elongation at break were observed for the base film in comparison to the naturally cooled composite film. The low degree of crystallinity and crystallite size in the ‘base film’ explain all of its mechanical and morphological properties. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 1427–1434, 2004     

Hybrid‐filler filled polypropylene/(natural rubber) composites: Effects of natural weathering on mechanical and thermal properties and morphology

Comparison was made between the properties of recycled newspaper (RNP)/carbon black (CB) and recycled newspaper (RNP)/silica hybrid filled polypropylene (PP)/natural rubber (NR) composites. The properties studied were mechanical, thermal, and morphological. These composites were also subjected to natural weathering, i.e., the tropical climate in Penang, Malaysia, for 6 months. The incorporation of CB and silica at all weight ratios of RNP/CB and RNP/silica hybrid gave increases in tensile strength, elongation at break (E_B), Young's modulus, melting temperature (T_m), heat of fusion of composites (ΔH_f(com)), crystallinity of composites (X_com), and the crystallinity of PP (X_PP). As expected, the tensile properties (except for Young's modulus), T_m, ΔH_f(com), X_com, and X_PP of the composites exhibited lower values after weathering than before weathering. The extent of chemical degradation was studied by Fourier transform infrared spectroscopy, and the results showed the formation of several functional groups, i.e., hydroxyl, hydroperoxide, vinyl, carboxylic acid, and ketone. At the same filler weight ratio, the composites filled with RNP/CB hybrid showed higher values of tensile strength and E_B but lower values of Young's modulus, ΔH_f(com), X_PP, and X_PP, as compared to those with the RNP/silica hybrid under weathering conditions. The good retention in tensile properties indicated that the replacement of RNP by CB and silica improved the weatherability performance of the PP/NR composites. J. VINYL ADDIT. TECHNOL., 2008. © 2008 Society of Plastics Engineers