Effect of printing parameters on mechanical properties of extrusion-based additively manufactured ceramic parts

The purpose of this study is to investigate the effect of printing parameters on the physical and mechanical properties of additively manufactured ceramics (alumina and zirconia). Sample parts were obtained by extrusion-based additive manufacturing of a ceramic-binder mixture and subsequent post-processing (debinding and sintering). Their mechanical properties (microhardness, flexural strength, toughness) were measured and correlated with the printing parameters. Part orientation is the most significant factor for microhardness and flexural strength in both ceramic materials. Parts with vertical orientation show higher hardness while horizontal samples show higher flexural strength compared to their respective counterparts. Extrusion velocity was found to be insignificant for hardness and flexural strength. However, a marginal increase in fracture toughness with the increase in the extrusion velocity was observed. The fracture toughness of additively manufactured ceramics shows an increasing trend with elastic modulus and flexural strength and a decreasing trend with hardness and sintered density.     

Kinetics of water absorption and hygrothermal aging rubber toughened poly(butylene terephthalate) with and without short glass fiber reinforcement

The objectives of this paper were to investigate the water absorption and hygrothermal aging behavior of rubber‐toughened poly(butylenes terephthalate) (RT‐PBT) with and without short glass fiber (SGF) reinforcement. The rubbers used in the study were AX8900 and EXL2314, both of which are acrylate‐based terpolymer. The effect of the hygrothermal aging on its fracture properties was also studied. The kinetics of the water absorption study were carried out on the injection‐molded samples of the RT‐PBTs and the SGF‐reinforced rubber‐toughened PBT (SGF‐RT‐PBT) at three immersion temperatures, 30, 60 and 90°C, for a total of 450 h. The study of the deterioration caused by the hygrothermal aging was conducted by investigating the fracture parameters and flexural properties of all the materials as both hygrothermally aged (HA) and redried state (RD). The modes of the failure of HA and RD samples were studied using the scanning electron microscopy (SEM) technique. It was found that all the samples conformed to Fickian behavior and the kinetics of absorption exhibited a strong dependency on the rubber types, presence of SGF, as well as the immersion temperature. Generally, SGF‐RT‐PBT showed a better resistance to hygrothermal aging than that of RT‐PBT and PBT, though a declining trend was observed in the fracture parameters, K_c and G_c. However, an opposite observation was exhibited in the flexural properties in some, but not all cases. Finally, the results obtained from SEM micrographs showed that permanent damage occurred in the materials and the hygrothermal aging had suppressed the plastic deformation ability of the PBT matrix and both types of impact modifiers where brittle failure was observed. Fiber pull‐out was apparently the failure mode of the SGF‐reinforced materials. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 506–516, 2004     

Controlling Crystallization: A Key Factor during 3D Printing with the Advanced Semicrystalline Polymeric Materials PEEK,PEKK 6002, and PEKK 7002

Controlling the crystallization of advanced, high-performance polymeric materials during 3D printing is critical to ensure that the resulting structures have appropriate mechanical properties. In this work, two grades of polyetherketoneketone (PEKK 6002 and PEKK 7002) are used to print 3D specimens via a fused filament fabrication process. The samples are compared with polyetheretherketone printed under the same conditions. Two approaches for controlling the crystallization process are undertaken. The first involves adjustment of the chamber temperature between room temperature and 190 °C to create two regions where crystallization is governed by the slow diffusion process and elevated by limiting the nucleation process. The second approach involves selection of PEKK materials with varying crystallization kinetics, namely. Application of this method into 3D-printing process allows for printing semicrystalline materials with tailored mechanical, thermal, and chemical properties as either amorphous or in situ crystallized products. The studies undertaken here provide the basis to eliminate expensive and time-consuming post-processing of 3D fabricated parts. In particular, solutions for the avoidance of poor adhesion to the building plate and weak interlayer adhesion that can lead to warping are described. The materials are divided into three groups, slow, moderate, and too fast crystallization kinetics.     

Mechanical Properties of Carbon Epoxy Prepreg Insert Phenolic Resin Injection Moldings

This study focuses on the insert-injection molding process. The thermoset composite inserts in this study were carbon fiber/epoxy(CF/Epoxy) prepreg sheets. The injected molded part was glass fiber contained phenolic resin(GF/PF). The CF/Epoxy was placed in the mold cavity prior to injecting GF/PF onto the inserted injection molded CF/Epoxy specimens. The role of adhesion between the inserted part and injected resin on the mechanical properties was evaluated by 3 point bending and impact tests. In addition, the effect of prepreg orientation on the mechanical properties of the prepreg inserted-injection molding system was investigated. It was found that the prepreg with unidirectional orientation significantly improved flexural and impact strength of the inserted injection molding composites, providing better support and resistance to bending and impact loading. The main failure modes of the specimens were structural and adhesive failure.     

Effects of electrophoretic deposition process parameters on the mechanical properties of graphene carboxyl-grafted carbon fiber reinforced polymer composite

Carbon fiber (CF) modification by grafting of various graphene-based nanofillers (GBN) by electrophoretic deposition (EPD) technique was proven to be a successful technique to enhance the out-of-plane performance of carbon fiber reinforced polymer (CFRP) composites. Graphene carboxyl (G-COOH) grafting on carbon fiber by electrophoretic deposition (EPD) is a promising technique to improve the mechanical properties of CFRP composites. To our knowledge, there is a dearth of literature available on the effect of EPD process parameters on the mechanical behavior of modified CFRP composites. The aim of this study is to evaluate the effect of nanofiller concentration in the suspension, applied current, and the time of deposition during EPD on the mechanical behavior of nanophase CFRP composites, thus making it a novel work. With increasing concentration, interlaminar shear strength (ILSS) improved consistently and has shown a maximum enhancement of 24.7% than that of neat CFRP composite at 1.5 g/L nanofiller concentration, whereas flexural strength remained almost unaffected with varying concentration. On the contrary, variation of deposition current has affected the flexural strength but not ILSS. The maximum flexural strength was obtained at a deposition current of 5.0A with an improvement of 16.3% in comparison with neat CFRP samples. However, both flexural strength and ILSS of hybrid CFRP composites have shown improvement with increasing deposition time. At 60 min of deposition, ILSS and flexural strength have shown maximum improvements of 35.0 and 26.6%, respectively, when compared to control specimen. After evaluating the effect of process parameters future scope of the work involves the optimization of parameters for EPD of G-COOH. Fractographic analysis of the fractured samples was performed using scanning electron microscope (SEM) to apprehend prominent failure mechanisms. © 2020 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48925.     

High Porosity Poly(ether ketone ketone): Influence of Solvents on Foam Properties

Poly(ether ketone ketone) (PEKK) is a semicrystalline high-performance polymer with exceptional mechanical properties, high continuous operation temperature, and is insoluble in most common solvents. Porous PEKK, desired for biomedical applications, is produced by a high-temperature thermally induced phase separation process using PEKK solutions in two high boiling aprotic solvents, 4-phenylphenol and 9-fluorenone, with concentrations up to 20 wt.%. It is demonstrated that the solvent choice has a pronounced influence on the phase separation behavior, which determines the foam morphology, physical and mechanical properties of PEKK foams. Porous PEKK with porosities ranging from 70% to 90%, specific surface areas up to 194 m² g⁻¹ and elastic moduli ranging from 35 to 100 MPa are produced.     

Evaluation of additively manufactured ultraperformance polymers to use as thermal protection systems for spacecraft

In this study, high-temperature thermoplastic polymers were three-dimensional (3D) printed and evaluated for ablation performances for the first time. The purpose of this study is to fabricate, test, and evaluate several ultraperformance thermoplastics, including polyetherimide (PEI), polyether ether ketone (PEEK), and poly(ether ketone ketone) (PEKK) for thermal, flammability, and ablation properties using fused filament fabrication. Among all tested materials, PEKK exhibit the highest char yield while the two PEEKs exhibit the highest decomposition temperature. Although PEI have the lowest onset decomposition temperature, microscale combustion calorimetry results indicate that it has the lowest heat release properties. For the 15 s oxyacetylene test bed (OTB) ablation test, all five materials experienced various amount of intumescent or swelling behavior. Samples after 30 s test experienced greater mass loss among which PEKK and ULTEM 9085 shows the highest char yield. Scanning electron microscopy microstructural analysis of the char and pyrolysis zones reveal highly porous char structures caused by the rapid generation of the volatile decomposition products. To fully exploit the experimental data provided by the OTB, the flowfield generated during aerothermal testing using this heat source was modeled. Computational fluid dynamics analysis using Ansys/Fluent 19.1 code was used to the heat transfer between the ablative surface and the combustion gases generated by the OTB and compared with experimental results.     

Impact of processing conditions and sizing on the thermomechanical and morphological properties of polypropylene/carbon fiber composites fabricated by material extrusion additive manufacturing

For the 3D printed composites, fiber alignment is affected by the direction of melt-flow during extrusion of filaments and subsequently through the printing nozzle. The resulting fibers orientation and the fiber-matrix compatibility have a direct correlation with mechanical properties. This study investigates the impact of processing conditions on the state of the carbon fiber types and their orientation on the mechanical properties of 3D-printed composites. Short and long carbon fibers were used as starting reinforcing materials, and the state of fibers at the beginning and on the printed parts were evaluated. Strong anisotropy in terms of mechanical properties (flexural and impact properties) was observed for the samples printed with different printing orientations. Interestingly, the number of voids in the printed composites was found to be correlated with the fiber types. The present work provides a step towards the optimization of tailored composite properties by additive manufacturing.     

Direct observation of the fracture behavior of the polyether ketone ketone (PEKK) spherulites

This article reports the direct observation of the fracture of individual poly-ether-ketone-ketone (PEKK) spherulites. A single layer of PEKK spherulites was obtained by bonding a PEKK film in-between two sandblasted Ti alloy plates using an autoclave. The crack of an individual PEKK spherulite was achieved by opening the Ti/PEKK/Ti sandwich using a double cantilever beam test. The fracture morphology of the PEKK spherulite was characterized using scanning electron microscopy and atomic force microscopy. It was found that under tensile stress the crack of the individual spherulite propagates along the middle plane and crosses the nucleation core. This is due to the symmetric radial structure of the spherulite. Moreover, it was found that the fracture surface morphology at the core of the spherulite is strongly influenced by the local crystalline structure, which is anisotropic and determined by the initial nucleation growth direction. As a result, the area fraction experiencing plastic deformation during the fracture of PEKK spherulites at different orientations may vary by an order of 10. Our results show the important role of the initial nucleation growth direction on the mechanical properties of the polymer crystals and may provide a new approach to the design of high-performance polymer materials with tailored crystalline structures.     

特种工程塑料聚醚酮酮的性能

采用国产化聚醚酮酮(PEKK)原料,应用差示扫描量热法、热失重分析法、X射线衍射法、傅立叶变换红外光谱仪等手段对PEKK的耐热性、加工性能、力学性能进行了表征与测量。测试结果显示,PEKK是半结晶聚合物,加工温度范围在360~380℃,热稳定性很好,热分解温度在500℃以上。通过测试获得了较详实的数据,为国产PEKK的工业化应用提供了加工依据。     

The influence of processing conditions on the mechanical properties of poly(aryl-ether-ketone)/polybenzimidazole blends

Interest in developing high-performance blends for niche applications has grown significantly in efforts to meet ever-increasing harsh environment demands. In this work, four model poly(aryl-ether-ketone)/polybenzimidazole (PAEK/PBI) blends were chosen to study the influence of premixing methods, processing, and matrix polymers, on their mechanical properties. Among the model poly(ether ether ketone) (PEEK) and PBI blends, mechanical properties are greatly enhanced by melt premixing. The molding process mainly affects the matrix crystallinity, which in turn greatly influences fracture toughness of the blend. Poly(ether ketone ketone) (PEKK) and PBI blend exhibits a slightly lower tensile strength and fracture toughness than PEEK/PBI due to the differences in inherent properties of PEEK and PEKK matrices and their interfacial interaction with PBI. The processing−structure–property relationship of PAEK/PBI blends is established to help guide optimal design of high-performance polymer blends for structural applications. © 2020 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48966.     

Thermal conductivity and diffusivity of carbon-reinforced polyetherketoneketone composites

Heat transfer properties play an important role in processing of polyetherketoneketone (PEKK)/carbon fiber (CF) composites. Accordingly, thermal conductivity and diffusivity of PEKK, PEKK/glassy carbon (GC), and PEKK/CF composites have been studied. Observed increase in conductivity and diffusivity with carbon filler addition was analyzed using the Maxwell–Eucken model. PEKK/GC composites with low carbon fraction indicated good fitting experimental points of the model, indicating good dispersion of particles. For PEKK/CF composites, the thermal conductivity and diffusivity increase is a reflection of a decrease in porosity. Results as observed from the model points to a homogenous dispersion within the PEKK/CF composites as well. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47975.     

Morphologies,Mechanical Properties and Wear of Poly(ether ketone ketone) (PEKK) and its Composites Reinforced with Mica

Poly(ether ketone ketone) (PEKK) composites were developed using mica as a filler. Sulfonated poly(ether ketone ketone) (S‐PEKK), a possible interfacial modifier, was coated on the mica surface with ca. 50 nm thickness, as observed by contact atomic force microscope (AFM). The morphologies of these materials were examined by scanning electron microscopy (SEM). In comparison with PEKK, significantly improved mechanical properties were obtained for the composite materials. With increasing content of mica in the materials, tensile modulus of the materials increased and ultimate elongation decreased. The composites containing 30 wt.‐% of mica exhibited a maximum tensile strength of about 200 MPa while pure PEKK showed a tensile strength of 102 MPa. The composites filled with mica treated by S‐PEKK displayed somewhat higher values of tensile strength and ultimate elongation than those generated using pure mica. The glass transition behavior and thermal stability of PEKK were not affected by the composition of the materials. The amount of mica used in the composites showed some influence on the coefficient of friction and wearing rate of these materials.     

Effect of Loading Rate and Surface Conditions on the Flexural Strength of Borosilicate Glass

This study evaluates the loading rate and surface condition dependence of the flexural strength of a borosilicate glass. The glass specimens are subjected to three different surface treatments before four-point bending tests to study the effect of surface flaws. Quasistatic (Material Test System 810) and dynamic (Kolsky bar) experiments are performed at loading rates ranging from 0.7 to 4 × 10⁶ MPa/s. The results show that the flexural strength of the borosilicate glass has a strong dependence on the loading rate. A chemically etched surface produces an enhanced flexural strength by about an order of magnitude. Scanning electron microscopy images on fracture surfaces indicate that the failure is governed by different types of flaws under different surface treatment conditions. Edge failure is also identified for samples possessing high flexural strength.     

Fatigue of glass fiber reinforced injection molded plastics. II: Tensile versus flexural loading

A previous paper reported fatigue data for several glass fiber reinforced thermoplastic materials by measuring their S-N, stress versus number of cycles to fail, behavior. It was demonstrated that both fiber orientation and loading mode, tensile versus flexural, strongly influence the resultant S-N data. The orientation effects are considered real, reflecting the local fiber orientation distributions in the samples, which are determined by geometry, processing and material variables. However, the higher fatigue lives observed in flexural loading are considered an artifact. Specifically for this class of materials, it is concluded that the use of linear elastic beam bending theory equations to calculate bending stresses are inappropriate. It is shown that a plasticity-based correction factor makes the flexural S-N data equivalent to the tensile results. In fact this correction applies equally well to monotonic loading, not just fatigue. Although it is concluded that tensile loading is preferred, some cases where flexural loading may be advantageous are indicated. Polym. Compos. 25:569–576, 2004. © 2004 Society of Plastics Engineers.     

Enhancement of Mechanical Properties of FDM‐PLA Parts via Thermal Annealing

The objective of this study is to investigate the possibility of enhancing mechanical properties of poly(lactic acid) (PLA) samples processed by a rapid manufacturing (RM) technique by increasing PLA crystallinity degree via thermal annealing. The samples are manufactured by fused deposition modeling (FDM) at different temperatures and subsequently evaluated by three‐point bending flexural and tensile tests. The polymer processed at 215 °C is thermally annealed over its glass transition temperature in order to increase the degree of crystallinity to the maximum attainable level as measured by the differential scanning calorimetry and confirmed by X‐ray diffraction. The increase in the degree of crystallinity of FDM‐PLA enhances flexural stress of the samples by 11–17%. The study also demonstrates applicability of radiation sterilization for FDM‐PLA parts. Therefore, thermal annealing might be introduced into a standard RM technology of PLA, particularly for sterilizable customized implants, to efficiently improve their mechanical properties.     

Interrelationship of strength and flow characteristics of polystyrene

This study investigated the interrelationship between strength and flow characteristics of general-purpose polystyrene (GPPS) used in injection molding applications. The ease of flow was chosen as a measure of processability and was evaluated using the melt flow rate and capillary rheometer techniques. Of the different strength tests that were examined, flexural and notched tensile strength tests were most effective in differentiating between commercial grades of high and low molecular weight GPPS. While characterizing strength of injection molded specimens, the degree of molecular orientation was taken into consideration. For unplasticized resins, increasing the weight average molecular weight by about 100,000 enhanced the flexural strength by 10%, but also increased the viscosity at low shear rates (10 to 100 s^?1). The increase in molecular weight had virtually no effect on viscosity at the highest shear rates (up to 10,000 s^?1). Plasticized resins displayed a 6% loss in flexural strength as well as a significant reduction in viscosity (throughout the shear rate range) as compared with the unplasticized resins. As expected, the improvement in strength achieved by increasing molecular weight leads to a simultaneous increase in the viscosity, i.e., a deterioration of processability. In addition, our study indicates that for samples without preferential molecular orientation, narrowing the molecular weight distribution significantly improves the balance of strength and melt flow rate properties.     

Impact of compression molding conditions on the thermal and mechanical properties of polyethylene

Compression molding is a current technique in polymer processing. Despite numerous studies, effect of molding pressure on physical properties has surprisingly not been fully investigated. In this study, the thermal and mechanical behavior of the compression‐molded polyethylene were thus explored to better grasp the relationship between processing parameters and ensuing properties. The effect of the molding temperature, pressure, cooling rate, and temperature profile on the tensile and flexural moduli as well as melting point of polyethylene was studied. We conclude that higher tensile and flexural moduli are obtained by increasing pressure and molding temperature, as well as decreasing the cooling rate. Our results were corroborated by X‐ray diffraction and differential scanning calorimetry measurements. Moreover, the use of a temperature gradient with different temperatures for the upper and bottom plates of the mold leads to asymmetric samples whose tensile and flexural moduli are improved. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46176.     

Study on mechanical properties and material distribution of sandwich plaques molded by co‐injection

In the sandwich injection molding process (co‐injection), two different polymer melts are sequentially injected into a mold to form a part with a skin/core structure. Sandwich molding can be used for recycling, improving barrier and electrical properties, or producing parts with tailored mechanical properties. In this study the evaluation of flexural modulus and impact strength of co‐injected plaques have been investigated. Virgin and short glass fiber reinforced (10 and 40%) polypropylene were used in six different combinations of sandwiched layers. The skin and core thicknesses were measured by optical microscopy and used to calculate the theoretical flexural modulus, which was compared to the experimentally measured modulus. Fiber orientation states were also observed by scanning electronic microscopy (SEM) at some specific locations and their effect on mechanical properties discussed. The experimental results indicate that an important improvement in transverse modulus, near the gate, is obtained when the virgin polypropylene (PP) is used as a skin and 40% short glass fiber polypropylene (PP40) as core. When both skin and core are made of PP40, the flexural moduli are slightly higher than conventionally injected PP40. POLYM. COMPOS. 26:265–275, 2005. © 2005 Society of Plastics Engineers.     

聚醚酮酮的合成与性能研究

在温和条件下,以1,2-二氯乙烷为溶剂、无水三氯化铝为催化剂、二苯醚和对苯二甲酰氯为原料合成了高分子量的聚醚酮酮(PEKK),并找到了用浓盐酸脱除催化剂、乙醇提纯聚合物的有效途径。测试了PEKK的主要物理和化学性能,其中PEKK的特性粘度可达0.8～1.0,达到了工程材料的要求。