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. 2022 Jun 9;14(12):2332.
doi: 10.3390/polym14122332.

Cenospheres-Reinforced PA-12 Composite: Preparation, Physicochemical Properties, and Soaking Tests

Damian S Nakonieczny  1   2 , Magdalena Antonowicz  2 , Thomas Heim  1 , Andrzej S Swinarew  3   4 , Paweł Nuckowski  5 , Krzysztof Matus  5 , Marcin Lemanowicz  6
Affiliations

Cenospheres-Reinforced PA-12 Composite: Preparation, Physicochemical Properties, and Soaking Tests

Damian S Nakonieczny et al. Polymers (Basel). .

Abstract

The main aim of this research was the preparation of a polymer-ceramic composite with PA-12 as the polymer matrix and modified aluminosilicate cenospheres (CSs) as the ceramic filler. The CSs were subjected to an early purification and cleaning process, which was also taken as a second objective. The CSs were surface modified by a two-step process: (1) etching in Piranha solution and (2) silanization in 3-aminopropyltriethoxysilane. The composite was made for 3D printing by FDM. Raw and modified CSs and a composite with PA-12 were subjected to the following tests: surface development including pores (BET), real density (HP), chemical composition and morphology (SEM/EDS, FTIR), grain analysis (PSD), phase composition (XRD), hardness (HV), and static tensile tests. The composites were subjected to soaking under simulated body fluid (SBF) conditions in artificial saliva for 14, 21, and 29 days. Compared to pure PA-12, PA-12_CS had generally better mechanical properties and was more resistant to SBF at elevated temperatures and soaking times. These results showed this material has potential for use in biomedical applications. These results also showed the necessity of developing a kinetic aging model for aging in different liquids to verify the true value of this material.

Keywords: APTES; Piranha solution; cenospheres; composites; polyamide PA-12; surface modification.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
The purification and modification process of CSs used in this study.
Figure 2
Figure 2
Sample type 1BA for strength tests.
Figure 3
Figure 3
The obtained, purified cenospheres’ fractions (energy: 20 keV), mag. 300×: (A) F_45, (B) F_90, (C) F_150, and (D) F_212.
Figure 4
Figure 4
SEM microphotographs of the CS fraction F_212 (energy: 20 keV): (A) SE mode, (B) BSE mode.
Figure 5
Figure 5
SEM microphotographs: CS fraction F_212 detail; we observed smaller CSs inside larger ones, mag. ×2770.
Figure 6
Figure 6
XRD patterns for raw CSs after purification: (A) F_45, (B) F_90, (C) F_150, (D) F_212.
Figure 6
Figure 6
XRD patterns for raw CSs after purification: (A) F_45, (B) F_90, (C) F_150, (D) F_212.
Figure 7
Figure 7
BJH–BET adsorption isotherms for F_45.
Figure 8
Figure 8
PSD results for raw CSs: (A) F_45, (B) CS—F_150, (C) CS—F _90, (D) CS—F_212.
Figure 9
Figure 9
SEM microphotographs for CS F_90 fraction (energy: 20 keV): (A) SE mode, (B) BSE mode.
Figure 10
Figure 10
EDS spectra for CS F_45 fraction (energy: 20 keV).
Figure 11
Figure 11
FTIR spectra for raw CSs: 45-F_45, 90-F_90, 150-F_150, and 212-F_212.
Figure 12
Figure 12
Comparison of FTIR spectra for 90-F_90 and 90_mod-M_90.
Figure 13
Figure 13
Young’s modulus, elongation at ultimate tensile strength, and ultimate tensile strength of the PA12 and PA12_CS in the initial state and after soaking in artificial saliva (SBF).
Figure 14
Figure 14
SEM microphotographs: breakthrough PA-12_CS samples: (A) SEM image, (B) image showing the marked inhomogeneous distribution of CSs in the matrix (concentrations of saturated pink color).
Figure 15
Figure 15
SEM microphotographs of breakthrough PA-12_CS samples: (A) CSs without a surface modification, (B) detail: surface of unmodified CSs, (C) CSs with surface modification, (D) detail: surface-modified CSs.
See this image and copyright information in PMC

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