Microstructural Effect of Extrusion-Blended PLA/BaTiO3 Composite: SEM and XRD Analysis
Notice bibliographique
Résumé
Polymer-ceramic composites are trending due to their exceptional strength-to-weight ratio, making them excellent candidates for various applications [1]. The aim of this study is to explore the microstructural properties that BaTiO3 can exhibit within a matrix of polylactic acid (PLA) undergoing an additive manufacturing process. The composite was prepared by extrusion mixing, with the main objective of fabricating the filaments that would be used to print a three-dimensional scaffold using triple periodic surface minimum geometry (TPMS) [2]. The model was generated using computational coding techniques, specifically, employing the Schwarz equation to generate a primitive porous scaffold using Python programming language coding (Fig. 1a). BTO-PLA composite was obtained by mixing 10 wt. % of BaTiO3 powder, 85 wt. % of PLA 4060D and 5 wt. % of glycerin. An extruder (Brabender Plasticorder) was used to produce a filament of 0.175 cm diameter, at a speed of 15 RPM, a die extrusion temperature of 155°C, and an extruder screw temperature of 140 °C. The morphological characteristics of the composite were analyzed by scanning electron microscopy (SEM), the global and punctual elemental analysis was performed by energy dispersive X-ray spectroscopy (EDS) and its structural characterization by X-ray diffraction (XRD). SEM micrographs taken from the cross-section of the filament were collected with a JEOL- JSM-7401F instrument. It was observed a rough texture for PLA accompanied by a distribution of agglomerated BaTiO3 particles (Fig. 1b-c). The global elemental mapping (EDX) confirms a dispersion of the BaTiO3 particles in the very homogeneous polymer matrix, highlighting the presence of Ba and Ti (Fig. 1d-g). The XRD pattern of the BTO-PLA composite was obtained in an X'Pert Pro diffractometer in the Bragg-Brentano geometry employing the Cu Kα radiation (λ = 1.5418 Å). The XRD pattern was refined through the Rietveld method using the FullProf software and the SH method. The lattice parameters obtained in this refinement were a = b = 3.999 Å and c = 4.026 Å (Figure 2a). The XRD pattern was indexed with PDF file No. 75-1606 associated with a perovskite-type structure with tetragonal phase and P4mm symmetry (No. 99). The crystal shape was elucidated using the GFourier program in a three-dimensional and a bidimensional (2D) view (Fig. 2b-c). A distinctive morphology of a quasi-cubic with prominent peaks can be observed. This crystal shape can be attributed to the inherent crystallographic structure of BaTiO3 combined with the constraints imposed by the PLA matrix during the formation of the composite. In addition, the extrusion process during filament preparation could have influenced the crystalline morphology. Extrusion introduces shear forces and mechanical stress, which can alter the orientation and shape of crystallites within the composite, potentially, contributing to the observed distortion. This morphology may have significant implications for the mechanical and piezoelectric properties of the composite, warranting further investigation. A BTO-PLA composite was successfully obtained through extrusion manufacturing. The BTO particles are homogeneously dispersed over the PLA matrix. The XRD analysis confirms a tetragonal phase and the elemental microanalysis confirms the presence of Ba, Ti, and O. This work also paves the way for further research into the potential applications of PLA/BaTiO3 composites in fields such as additive manufacturing, biomedical engineering and electronics [3-5]. Furthermore, the use of TPMS geometry in composite fabrication offers unique opportunities for the design of tailored materials, aiming to improve mechanical properties and allowing the exploration of new functionalities [6]. (a) Design of BTO/PLA composite scaffold, (b) Cross-section SEM micrograph with magnification of 500x and (c) x1000 of BTO/PLA filament, while images (d-h) show the elemental mapping for Ba, Ti, O. (a) XRD Rietveld refinement of the extruded composite, (b) average crystallite shape in 2D obtained with GFourier software using SH method, and (c) apparent crystallite (quasi-cubic) shape for BTO/PLA composite after the extrusion process.
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Prédiction machine sur la base complète
Imitation des enseignantsNi prévalence calibrée, ni vérité terrain. Validation humaine à venir. Le volet Gemma est une étiquette directe du modèle pour chaque travail de la base, lue sur la notice réduite au titre. Le volet Codex est un classifieur appris des 10 348 étiquettes directes de Codex et calibré sur les taux pondérés de l'échantillon; les champs sans appui suffisant ne portent aucun appel Codex. Le mode candidate est l'union des deux volets; le consensus est leur intersection. Ces sorties portent le statut machine_predicted_unvalidated et ne sont pas des étiquettes humaines.
Scores du classifieur distillé par catégorie (deux têtes)
| Catégorie | Codex | Gemma |
|---|---|---|
| Métarecherche | 0,000 | 0,000 |
| Méta-épidémiologie (sens strict) | 0,000 | 0,000 |
| Méta-épidémiologie (sens large) | 0,000 | 0,000 |
| Bibliométrie | 0,000 | 0,000 |
| Études des sciences et des technologies | 0,000 | 0,000 |
| Communication savante | 0,000 | 0,000 |
| Science ouverte | 0,000 | 0,000 |
| Intégrité de la recherche | 0,000 | 0,001 |
| Charge utile insuffisante (le modèle a refusé de juger) | 0,003 | 0,000 |
Scores machine (provisoires)
Les deux têtes enseignantes du modèle étudiant, lues sur ce travail. Un score ordonne la base pour la relecture; il n'affirme jamais une catégorie, et le statut de validation accompagne chaque rangée tel quel.
Scores de référence d'un modèle non mature (critères de maturité non atteints, 7 itérations). Un score ordonne; il n'affirme jamais une catégorie.
score_only:v0-immature-baseline · tel quel depuis la passe de notation : score_only signifie que le nombre peut ordonner les travaux, et qu'aucune étiquette de catégorie n'en découleClassification
machine, non validéePrédiction automatique; un appel candidat d’une seule source (Gemma direct ou Codex distillé), pas un consensus.
Le détail, modèle par modèle et score par score, se trouve en fin de page sous « Comment cette classification a été obtenue ».