“…However, as seen Figure S5b the bands that became weaker after phosphoric acid modification (954 and 970 cm –1 ) became more intense at 954 and 978 cm –1 wavelength after silane A-174 addition. Previous studies stated that band positioned at 978 cm –1 reveals the P–O–Si bonds. , …”
Section: Resultsmentioning
confidence: 97%
“…P–O–Si and Si–OH bond formations at HAP surface upon surface treatment are predicted by new XPS (O 1s) peak detected at around 532 eV and filamentous surface micromorphology observed in SEM images for HAPSi3 (Figure S7c). ,,, A new FTIR band at 978 cm –1 and a new XPS (O 1s) peak around 532 eV and a (P 2p) peak at 138 eV (β-TCPPASi3) also show that the P–O–Si and Si–OH bonds might have formed after silane A-174 treatment of β-TCP. ,, …”
Section: Discussionmentioning
confidence: 96%
“…Also, β-TCPPASi3 displays an additional band at 138 eV (P 2p) with low intensity. It should be noted that FTIR spectra of β-TCPPASi1 and β-TCPPASi3 exhibited a feature at 978 cm −1 , which was attributed to newly formed P−O−Si bonds 2,46 Therefore, this new P 2p peak of β-TCPPASi3 at 138 eV could be associated with P−O−Si bonds. This feature is not observed inP 2p spectrum of β-TCPPASi1, possibly due to much lower amount of silane A-174 on surface.…”
Section: Bulk Structural Characteristics Of Raw Materials and Silanementioning
confidence: 96%
“…Previous studies stated that band positioned at 978 cm −1 reveals the P−O−Si bonds. 2,46 Figure S6 demonstrates the FTIR spectrum of PLA. The feature positioned at 872 cm −1 corresponds to C−COO stretching vibrations.…”
Section: Bulk Structural Characteristics Of Raw Materials and Silanementioning
The effect of silane A-174 (3-(trimethoxysilyl)propyl methacrylate (methacryloxypropyl trimethoxysilane)) modifications of the ceramic surface on the structural characteristics and mechanical performance of hydroxyapatite (HAP)−polylactic acid (PLA) and β-tricalcium phosphate (β-TCP)−PLA composite systems was investigated employing a combination of Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), compressive strength measurements, and statistical models constructed via projection to latent structures (PLS) analysis. The composites were synthesized by solvent casting method at ambient conditions employing ceramic/PLA ratios of 60/40 and 50/ 50, and silane A-174 percentages of 0, 1, and 3 wt %. Peak positions of O 1s, Ca 2p, P 2p, Si 2p, and C 1s in XP spectra of ceramics, surface-modified ceramics, and the corresponding composites and compressive strength values were used as the predictors and response variables in PLS models. It was found that Ca 2p, P 2p, and Si 2p binding energies of the ceramic component employed in composite synthesis played the most significant role in determining compressive strength. PLA-HAP composite with a ceramic/PLA ratio of 50/50, synthesized employing 3 wt % silane A-174 treated HAP (HAP50PLA50Si3), resulted in enhancement of the compressive strength up to 365 MPa, which is the highest compressive strength value reported in the literature to the best of our knowledge. Additional P 2p, Ca 2p, and C 1s features positioned at 129.64, 350.08, and 280.74 eV in the XP spectra of this specimen together with significant shifts of Si 2p and C 1s bands toward lower binding energies and polymer-bridge-like surface characteristics signaled improved polymer−ceramic interaction in this composite. Attaining mechanical performance comparable with and even higher than that of cortical bone upon silane A-174 modifications might provide opportunities for clinical applications toward developing bioresorbable PLA-HAP-based implants that can be employed in load-bearing applications such as knee and hip replacements.
“…However, as seen Figure S5b the bands that became weaker after phosphoric acid modification (954 and 970 cm –1 ) became more intense at 954 and 978 cm –1 wavelength after silane A-174 addition. Previous studies stated that band positioned at 978 cm –1 reveals the P–O–Si bonds. , …”
Section: Resultsmentioning
confidence: 97%
“…P–O–Si and Si–OH bond formations at HAP surface upon surface treatment are predicted by new XPS (O 1s) peak detected at around 532 eV and filamentous surface micromorphology observed in SEM images for HAPSi3 (Figure S7c). ,,, A new FTIR band at 978 cm –1 and a new XPS (O 1s) peak around 532 eV and a (P 2p) peak at 138 eV (β-TCPPASi3) also show that the P–O–Si and Si–OH bonds might have formed after silane A-174 treatment of β-TCP. ,, …”
Section: Discussionmentioning
confidence: 96%
“…Also, β-TCPPASi3 displays an additional band at 138 eV (P 2p) with low intensity. It should be noted that FTIR spectra of β-TCPPASi1 and β-TCPPASi3 exhibited a feature at 978 cm −1 , which was attributed to newly formed P−O−Si bonds 2,46 Therefore, this new P 2p peak of β-TCPPASi3 at 138 eV could be associated with P−O−Si bonds. This feature is not observed inP 2p spectrum of β-TCPPASi1, possibly due to much lower amount of silane A-174 on surface.…”
Section: Bulk Structural Characteristics Of Raw Materials and Silanementioning
confidence: 96%
“…Previous studies stated that band positioned at 978 cm −1 reveals the P−O−Si bonds. 2,46 Figure S6 demonstrates the FTIR spectrum of PLA. The feature positioned at 872 cm −1 corresponds to C−COO stretching vibrations.…”
Section: Bulk Structural Characteristics Of Raw Materials and Silanementioning
The effect of silane A-174 (3-(trimethoxysilyl)propyl methacrylate (methacryloxypropyl trimethoxysilane)) modifications of the ceramic surface on the structural characteristics and mechanical performance of hydroxyapatite (HAP)−polylactic acid (PLA) and β-tricalcium phosphate (β-TCP)−PLA composite systems was investigated employing a combination of Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), compressive strength measurements, and statistical models constructed via projection to latent structures (PLS) analysis. The composites were synthesized by solvent casting method at ambient conditions employing ceramic/PLA ratios of 60/40 and 50/ 50, and silane A-174 percentages of 0, 1, and 3 wt %. Peak positions of O 1s, Ca 2p, P 2p, Si 2p, and C 1s in XP spectra of ceramics, surface-modified ceramics, and the corresponding composites and compressive strength values were used as the predictors and response variables in PLS models. It was found that Ca 2p, P 2p, and Si 2p binding energies of the ceramic component employed in composite synthesis played the most significant role in determining compressive strength. PLA-HAP composite with a ceramic/PLA ratio of 50/50, synthesized employing 3 wt % silane A-174 treated HAP (HAP50PLA50Si3), resulted in enhancement of the compressive strength up to 365 MPa, which is the highest compressive strength value reported in the literature to the best of our knowledge. Additional P 2p, Ca 2p, and C 1s features positioned at 129.64, 350.08, and 280.74 eV in the XP spectra of this specimen together with significant shifts of Si 2p and C 1s bands toward lower binding energies and polymer-bridge-like surface characteristics signaled improved polymer−ceramic interaction in this composite. Attaining mechanical performance comparable with and even higher than that of cortical bone upon silane A-174 modifications might provide opportunities for clinical applications toward developing bioresorbable PLA-HAP-based implants that can be employed in load-bearing applications such as knee and hip replacements.
“…Figure 2 displays the solid-state 29 Si NMR spectrum of the silicon coating. The silicate units are usually represented by Q n , referring to a silicon with n bridging oxygens to other silicon atoms [ 33 , 34 ]. For the solid-state 29 Si NMR spectrum, the signals are located between −100 and −120 ppm, which indicates the presence of a 29 Si nucleus in a tetrahedral oxygen environment.…”
This paper aims to develop a novel method, i.e., sol-gel combined with layer-by-layer assembly technology, to impart flame retardancy on polyacrylonitrile (PAN) fabrics. Silica-sol was synthesized via the sol-gel process and acted as cationic solution, and phytic acid (PA) was used as the anionic medium. Flame-retardant-treated PAN fabric (FR-PAN) could achieve excellent flame retardancy with 10 bilayer (10BL) coating through layer-by-layer assembly. The structure of the fabrics was characterized by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). The thermal stability and flame retardancy were evaluated by thermogravimetric (TG) analysis, cone calorimetry (CC) and limiting oxygen index (LOI). The LOI value of the coated fabric was up to 33.2 vol % and the char residue at 800 °C also increased to 57 wt %. Cone calorimetry tests revealed that, compared to the control fabric, the peak of heat release rate (PHRR) and total heat release (THR) of FR-PAN decreased by 66% and 73%, respectively. These results indicated that sol-gel combined with layer-by-layer assembly technique could impart PAN fabric with satisfactory flame-retardant properties, showing an efficient flame retardant strategy for PAN fabric.
Materials based on silicon-phosphorus mixed oxides have traditionally attracted interest in electronics, optics, catalysis, and related fields. The preparation of a solid containing stable Si–O–P linkages is a huge challenge due to their intrinsic instability to hydrolysis in a wet atmosphere. On the other hand, most technological applications of these materials, such as protonic conductive membranes in fuel cells and water-tolerant solid acid catalysts, are related to their interaction with water; consequently, suitable synthesis procedures that positively face this tradeoff are mandatory. Besides the traditional high-temperature techniques, sol-gel synthetic methods represent a viable, low-cost alternative, allowing for the preparation of high-purity materials with a homogeneous distribution of the components at the atomic scale. Si–O–P linkages are easily obtained by nonhydrolytic sol-gel routes, but only in inert and dry atmosphere. Conversely, hydrolytic routes offer opportunities to control the structure of the products in a wide range of processing conditions. The present review aims at providing an overall picture of the research on the sol-gel synthesis of phosphosilicate and related materials and theisr different applications, emphasizing how the interest in these systems is still lively, considering both conventional and emerging applications, such as flame retardance. The incorporation of Si–O–P nanostructures in polymer composites, coatings, and textiles is indeed a promising strategy to improve properties like thermal stability and fire resistance; however, their in-situ synthesis brings about additional difficulties related to the reactivity of the precursors. The perspectives linked with the development of Si–P-based materials are finally outlined.
Graphical Abstract
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