Phosphate Glass Fiber Research Articles

Synthesis and characterization of new continuous phosphate glass fibers intended for structural engineering applications: Structure/property relationships

Nowadays, phosphate glass fibers (PGF) are considered quite competitive respective to conventional glass fibers. This work focus on the development of PGF fibers intended for structural engineering applications such as composite reinforcement for building and automotive fields. For this purpose, two series of phosphate glasses based on 52P2O5-24CaO-13MgO-(11-(X+Y+Z)) K2O-XAL2O3-YF2O3-ZTiO2; (X=1; 3; 5, Y=0; 5, Z=0; 1 mol %) were processed and transformed into phosphate glass fibers by melt spinning. The resulting fibers were characterized. XRD analysis confirmed the non-crystalline nature of phosphate glasses. In addition, the substitution of K2O by Al2O3 and by the combination of Al2O3, Fe2O3 and TiO2 in the composition of phosphate glass could lead to a significant increase in fiber density from 2,16 g/cm3 to 2,80 g/cm3. The stability of the produced phosphate glass fibers was examined using two methods: weight loss at 37°C and dissolution kinetics under different pH levels (4, 7, and 12). The results showed that the chemical resistance of the PGF fibers was improved with up to 99% increase respective to the original formulation. In addition, the mechanical properties of the spinnable phosphate glass manufactured by replacing K2O oxide by Al2O3 oxide were improved, such a substitution led to a maximum tensile strength and modulus of 2668 MPa and 140 GPa, respectively. Therefore, the tensile proprieties were improved by 75% compared to the original formulation. This comparative study between phosphate glass fibers (PGF) and traditional fibers highlight similar tensile strength but combined to notable enhancements in chemical stability through cation addition, expanding their potential use in composite and biomedical materials. Finally, a correlation analysis of mechanical performances was carried out. It was observed that the results obtained using the statistical methods were consistent with the experimental data.

Multi-scale analysis of randomly reinforced polyester composites with short phosphate glass fibers: experimental insights and kinematic homogenization modeling

Multi-scale analysis of randomly reinforced polyester composites with short phosphate glass fibers: experimental insights and kinematic homogenization modeling

Enhanced highly bismuth‐doped multicomponent phosphate glass fibers for broadband amplifiers

AbstractBismuth (Bi)‐doped glass fibers are being developed into next‐generation broadband amplifiers and tunable lasers. Yet, the well‐developed Bi‐doped fiber devices only realize silica‐based optical fibers prepared by the modified chemical vapor deposition method, which faces challenges such as low doping concentration, high cost, intricate device structure, and high preparation difficulty. Here, a novel highly Bi‐doped multicomponent phosphate glass was developed. The high ion solubility of this phosphate glass facilitates achieving a Bi doping concentration of 8 mol%. The introduction of aluminum nitride (a new reducing agent) can create a local reducing environment, further increasing the concentration of low‐valence near‐infrared (NIR) active Bi ions. Furthermore, the resulting enhanced highly Bi‐doped multicomponent phosphate glass with efficient 900–1600 nm NIR emission can be drawn into corresponding optical fibers by a rod‐in‐tube method. Broadband NIR amplified spontaneous emission with a 3 dB bandwidth of 275 nm was achieved in this new fiber. As far as we know, this is the first successful preparation of Bi‐doped multicomponent phosphate glass fiber. Our results indicate that this fiber will be a powerful alternative to Bi‐doped silica‐based fibers for the preparation of related Bi‐doped fiber devices.

Use of bioresorbable fibers for short-wave infrared spectroscopy using time-domain diffuse optics.

We demonstrate the usability of bioresorbable phosphate glass fibers for time-domain diffuse optical spectroscopy (TD-DOS) in the short-wave infrared (SWIR) region of 950-1600 nm, with the use of an InGaAs detector. Bioresorbable fibers for diffuse optics present an exciting prospect due to their ability to be left implanted while retrieving optical properties from deeper regions (few cm) for monitoring treatments. Extending TD-DOS to the SWIR region could be useful to better identify biomarkers such as water, lipids and collagen, given their increase in absorption in this range. We attempt to use the bioresorbable fibers to spectrally identify these biomarkers by measuring a series of biological samples known to contain them, such as porcine muscle, porcine fat and bone. We further validate our measurements by comparing the optical properties of high-scattering solid silicone phantoms retrieved with these bioresorbable fibers with those by a standard Si fiber.

A phosphate glass reinforced composite acrylamide gradient scaffold for osteochondral interface regeneration

The bone-cartilage interface is defined by a unique arrangement of cells and tissue matrix. Injury to the interface can contribute to the development of arthritic joint disease. Attempts to repair osteochondral damage through clinical trials have generated mixed outcomes. Tissue engineering offers the potential of integrated scaffold design with multiregional architecture to assist in tissue regeneration, such as the bone-cartilage interface. Challenges remain in joining distinct materials in a single scaffold mass while maintaining integrity and avoiding delamination. The aim of the current work is to examine the possibility of joining two closely related acrylamide derivatives such as, poly n-isopropyl acrylamide (pNIPAM) and poly n‑tert‑butyl acrylamide (pNTBAM). The target is to produce a single scaffold unit with distinct architectural regions in the favour of regenerating the osteochondral interface. Longitudinal phosphate glass fibres (PGFs) with the formula 50P2O5.30CaO.20Na2O were incorporated to provide additional bioactivity by degradation to release ions such as calcium and phosphate which are considered valuable to assist the mineralization process. Polymers were prepared via atom transfer radical polymerization (ATRP) and solutions cast to ensure the integration of polymers chains. Scaffold was characterized using scanning electron microscope (SEM) and Fourier transform infra-red (FTIR) techniques. The PGF mass degradation pattern was inspected using micro computed tomography (µCT). Biological assessment of primary human osteoblasts (hOBs) and primary human chondrocytes (hCHs) upon scaffolds was performed using alizarin red and colorimetric calcium assay for mineralization assessment; alcian blue staining and dimethyl-methylene blue (DMMB) assay for glycosaminoglycans (GAGs); immunostaining and enzyme-linked immunosorbent assay (ELISA) to detect functional proteins expression by cells such as collagen I, II, and annexin A2. FTIR analysis revealed an intact unit with gradual transformation from pNIPAM to pNTBAM. SEM images showed three distinct architectural regions with mean pore diameter of 54.5 µm (pNIPAM), 16.5 µm (pNTBAM) and 118 µm at the mixed interface. Osteogenic and mineralization potential by cells was observed upon the entire scaffold's regions. Chondrogenic activity was relevant on the pNTBAM side of the scaffold only with minimal evidence in the pNIPAM region. PGFs increased mineralization potential of both hOBs and hCHs, evidenced by elevated collagens I, X, and annexin A2 with reduction of collagen II in PGFs scaffolds. In conclusion, pNIPAM and pNTBAM integration created a multiregional scaffold with distinct architectural regions. Differential chondrogenic, osteogenic, and mineralized cell performance, in addition to the impact of PGF, suggests a potential role for phosphate glass-incorporated, acrylamide-derivative scaffolds in osteochondral interface regeneration.

Wound Healing Promotion via Release of Therapeutic Metallic Ions from Phosphate Glass Fibers: An In Vitro and Ex Vivo Study.

Biomaterials capable of promoting wound healing and preventing infections remain in great demand to address the global unmet need for the treatment of chronic wounds. Phosphate-based glasses (PG) have shown potential as bioresorbable materials capable of inducing tissue regeneration, while being replaced by regenerated tissue and releasing therapeutic species. In this work, phosphate-glass-based fibers (PGF) in the system P2O5-CaO-Na2O added with 1, 2, 4, 6, and 10 mol % of the therapeutic metallic ions (TMI) Ag+, Zn2+, and Fe3+ were manufactured via electrospinning of coacervate gels. Coacervation is a sustainable, cost-effective, water-based method to produce PG. All TMI are effective in promoting wound closure (re-epithelialization) in living human skin ex vivo, where the best-performing system is PGF containing Ag+. In particular, PGF with ≥4 mol % of Ag+ is capable of promoting 84% wound closure over 48 h. These results are confirmed by scratch test migration assays, with the PGF-Ag systems containing ≥6 mol % of Ag+, demonstrating significant wound closure enhancement (up to 72%) after 24 h. The PGF-Ag systems are also the most effective in terms of antibacterial activity against both the Gram-positive Staphylococcus aureus and the Gram-negative Escherichia coli. PGF doped with Zn2+ shows antibacterial activity only against S. aureus in the systems containing Zn2+ ≥ 10 mol %. In addition, PGF doped with Fe3+ rapidly accelerates ex vivo healing in patient chronic wound skin (>30% in 48 h), demonstrating the utility of doped PGF as a potential therapeutic strategy to treat chronic wounds.

Lithium-loaded GelMA-Phosphate glass fibre constructs: Implications for astrocyte response.

Combinations of different biomaterials with their own advantages as well as functionalization with other components have long been implemented in tissue engineering to improve the performance of the overall material. Biomaterials, particularly hydrogel platforms, have shown great potential for delivering compounds such as drugs, growth factors, and neurotrophic factors, as well as cells, in neural tissue engineering applications. In central the nervous system, astrocyte reactivity and glial scar formation are significant and complex challenges to tackle for neural and functional recovery. GelMA hydrogel-based tissue constructs have been developed in this study and combined with two different formulations of phosphate glass fibers (PGFs) (with Fe3+ or Ti2+ oxide) to impose physical and mechanical cues for modulating astrocyte cell behavior. This study was also aimed at investigating the effects of lithium-loaded GelMA-PGFs hydrogels in alleviating astrocyte reactivity and glial scar formation offering novel perspectives for neural tissue engineering applications. The rationale behind introducing lithium is driven by its long-proven therapeutic benefits in mental disorders, and neuroprotective and pronounced anti-inflammatory properties. The optimal concentrations of lithium and LPS were determined in vitro on primary rat astrocytes. Furthermore, qPCR was conducted for gene expression analysis of GFAP and IL-6 markers on primary astrocytes cultured 3D into GelMA and GelMA-PGFs hydrogels with and without lithium and in vitro stimulated with LPS for astrocyte reactivity. The results suggest that the combination of bioactive phosphate-based glass fibers and lithium loading into GelMA structures may impact GFAP expression and early IL-6 expression. Furthermore, GelMA-PGFs (Fe) constructs have shown improved performance in modulating glial scarring over GFAP regulation.

Bioactive Glass and Silica Particles for Skeletal and Cardiac Muscle Tissue Regeneration.

When skeletal and cardiac tissues are damaged, surgical approaches are not always successful and tissue regeneration approaches are investigated. Reports in the literature indicate that silica nanoparticles and bioactive glasses (BGs), including silicate bioactive glasses (e.g., 45S5 BG), phosphate glass fibers, boron-doped mesoporous BGs, borosilicate glasses, and aluminoborates, are promising for repairing skeletal muscle tissue. Silica nanoparticles and BGs have been combined with polymers to obtain aligned nanofibers and to maintain controlled delivery of nanoparticles for skeletal muscle repair. The literature indicates that cardiac muscle regeneration can be also triggered by the ionic products of BGs. This was observed to be due to the release of vascular endothelial growth factor and other growth factors from cardiomyocytes, which regulate endothelial cells to form capillary structures (angiogenesis). Specific studies, including both in vitro and in vivo approaches, are reviewed in this article. The analysis of the literature indicates that although the research field is still very limited, BGs are showing great promise for muscle tissue engineering and further research in the field should be carried out to expand our basic knowledge on the application of BGs in muscle (skeletal and cardiac) tissue regeneration. Impact statement This review highlights the potential of silica particles and bioactive glasses (BGs) for skeletal and cardiac tissue regeneration. These biomaterials create scaffolds triggering muscle cell differentiation. Ionic products from BGs stimulate growth factors, supporting angiogenesis in cardiac tissue repair. Further research is required to expand our know-how on silica particles and BGs in muscle tissue engineering.

Efficient laser operation with low loss Nd3+-doped phosphate glass fiber under direct pumping

For the first time, we have demonstrated efficient 1054 nm laser output with low loss Nd3+-doped phosphate glass fibers at room temperature using an 888 nm laser diode as the direct pumping source. Therein, the home-made Nd3+-doped phosphate glass fiber is the key for laser performance improvement. The transmission loss of the large-core single-cladding Nd3+-doped phosphate fibers prepared by the novel peeled-off isolated stacked extrusion method is as low as 1.1 dB/m at ∼1 μm. On this basis, a low-loss Fabry-Perot cavity is constructed by precisely controlling the relative distance between the fiber end facet and the cavity mirror with a microscope. The record-breaking optical-to-optical efficiency of Nd3+-doped phosphate glass fiber lasers, 50.2% is achieved with the maximum output power of 6.71 W. During laser operation, the output laser power does not roll over, even at high pump powers. The output laser power is limited only by the available pump power. This work will lay a solid foundation to the high-power fiber laser fabrication, and will find many applications in the future.

Biodegradable glass fiber reinforced PVA hydrogel for cartilage repair: mechanical properties, ions release behavior and cell recruitment

Articular cartilage with limited ability of regeneration remains a grand challenge in the field of tissue engineering. Poly(vinyl alcohol) (PVA) hydrogel with low friction coefficient have been regarded as prior candidate for cartilage substitute, whereas lack of structure performance and bioactivity limited their application. Phosphate glass fiber (PGF) with outstanding mechanical performance and nature of biodegradability presents potential capability to improve mechanical stability of hydrogel and chondrocyte metabolism as well as cell recruitment. Herein, we describe a novel PGF-PVA composites hydrogel incorporated with continuous PGF. The presence of stiff PGF not only improves the mechanical properties of hydrogel with maximum tensile strength of 12.44 MPa and Young's modulus of 68.35 MPa, but also endows the hydrogel molecular structure with the increase of crystallinity and thermal stability via formation of crosslinking points. More importantly, the PVA hydrogel matrix exhibits efficient ions exchange behavior to control ions concentration during PGF degradation, resulting in more suitable metabolic environment for chondrocyte proliferation and induction with enhanced recruitment. Therefore, it is believed that this work provides a kind of fiber reinforced hydrogel material promising excellent properties for cartilage repair.

Development and Characterization of Phosphate Glass Fibers and Their Application in the Reinforcement of Polyester Matrix Composites.

This study focused on the production and characterization of phosphate glass fibers (PGF) for application as composite reinforcement. Phosphate glasses belonging to the system 52P2O524CaO13MgO (11-(X + Y)) K2OXFe2O3YTiO2 (X:1, 3, 5) and (Y:0.5, 1) were elaborated and converted to phosphate glass fibers. First, their mechanical properties and chemical durability were investigated. Then, the optimized PGF compositions were used afterward as reinforcement for thermosetting composite materials. Polyester matrices reinforced with short phosphate glass fibers (sPGF) up to 20 wt % were manufactured by the contact molding process. The mechanical and morphological properties of different sPGF-reinforced polyester systems were evaluated. The choice between the different phosphate-based glass syntheses (PGFs) was determined by their superior mechanical performance, their interesting chemical durability, and their high level of dispersion in the polyester matrix without any ad sizing as proven by SEM morphological analysis. Moreover, the characterization of mechanical properties revealed that the tensile and flexural moduli of the developed polyester-based composites were improved by increasing the sPGF content in the polymer matrix in perfect agreement with Takayanagi model predictions. The present work thus highlights some promising results to obtain high-quality phosphate glass fiber-reinforced polyester parts which can be transposed to other thermosetting or thermoplastic-based composites for high-value applications.

L-DOPA coating improved phosphate glass fibre strength and fibre/matrix interface

The levodopa (L-DOPA) has been reported as a promising adhesive for various materials. In this study, we utilized L-DOPA as an interfacial agent for phosphate glass fibre/polycaprolactone (PGF/PCL) composites, with the aim to enhance the interfacial properties between the fibres and polymer matrix. The PGFs were dip-coated in varying concentrations of L-DOPA solution ranging between 5 and 40 g L-1. The fibre strength and interfacial shear strength (IFSS) of the composites were measured via a single fibre tensile test and single fibre fragmentation test, respectively. It was found that the L-DOPA agent (at conc. 10 g L-1) significantly improved the IFSS of the composites up to 27%. Also, the L-DOPA coating (at conc. 40 g L-1) significantly increased the glass fibre strength up to 18%. As a result, an optimum coating level could be tailored depending on application and whether fibre strength or IFSS was of greater importance. In addition, SEM and TGA analyses were used to detect and quantify the coating agents. FTIR and XPS further confirmed presence of the coating and indicated the zwitterionic crystals of L-DOPA and the formation of a melanin-like polymer layer. The spectroscopy data also evidenced that both catechol and amine groups contributed to the interaction between the L-DOPA and the PGF surface.

Ultrafast fiber laser at 0.9 µm with a gigahertz fundamental repetition rate by a high gain Nd3+-doped phosphate glass fiber.

Fiber lasers, owing to the advantages of excellent beam quality and unique robustness, play a crucial role in lots of fields in modern society. Developing optical glass fibers with superior performance is of fundamental importance for wide applications of fiber lasers. Here, a new Nd3+-doped phosphate single-mode fiber that enables a high gain at 0.9 µm is designed and fabricated. Compared to previous Nd3+-doped silica fibers, the developed phosphate fiber exhibits a significant gain promotion, up to 2.7 dB cm-1 at 915 nm. Configuring in a continuous-wave fiber laser, this phosphate fiber can provide a slope efficiency of 11.2% in a length of only 4.5 cm, about 6 times higher than that of Nd3+-doped silica fiber. To showcase its uniqueness, an ultrafast fiber laser with ultrashort cavity is constructed, such that an ultrashort pulse train with a fundamental repetition rate of up to 1.2 GHz is successfully generated. To the best of our knowledge, this is the highest fundamental repetition rate for mode-locked fiber lasers at this wavelength range - two orders of magnitude higher than that of prior works. These results indicate that this Nd3+-doped phosphate fiber is an effective gain medium for fiber amplifiers and lasers at 0.9 µm, and it is promising for two-photon biophotonics that requires long-term operation with low phototoxicity.

Spatial beam reshaping and large-band nonlinear conversion in rectangular-core phosphate glass fibers

Here we present the ability of Nd3+-doped zinc-phosphate glasses to be shaped into rectangular core fibers. At first, the physico-chemical properties of the developed P2O5-based materials are investigated for different concentrations of neodymium oxide and core and cladding glass compositions are selected for further fiber development. A modified stack-and-draw technique is used to produce multimode large rectangular-core optical fibers. Self-guided nonlinear effects acting as spatial beam reshaping processes occurring in these newly-developed photonic structures lead to the generation of spectral broadenings in the visible and near-infrared spectral domains.Graphic

Effect of Eu3+ and Tb3+ ions concentration on the mechanical, structural, and photoluminescence properties of phosphate glass fibers

Two series of phosphate glasses belonging to the (65-x) P2O5–35CaO–xRE2O3 system (RE = Eu or Tb; 0 ≤ x ≤ 6 mol%) were prepared by the melt-quenching technique. All compositions were successfully drawn as continuous monofilaments fibers. The effect of Eu3+ and Tb3+ ions concentration on their mechanical, structural, and photoluminescence properties was investigated. The results revealed that the highest tensile strength was 1031 ± 34 MPa for fibers doped with 6 mol% of Eu2O3 and 1014 ± 65 MPa for fibers doped with 6 mol% of Tb2O3. The addition of RE2O3 showed an increase in density and Tg. A structural investigation was carried out using FTIR spectroscopy. The photoluminescence properties in terms of excitation and emission spectra were investigated in detail. The most intense emission band at 611 nm corresponds to the 5D0 → 7F2 transition of Eu3+ ions under 392 nm excitation was observed for fibers doped with 6 mol% of Eu2O3. The most intense emission band at 543 nm corresponds to the 5D4 → 7F5 transition of Tb3+ ions under 374 nm excitation was observed for fibers doped with 6 mol% of Tb2O3. These two compositions exhibited the highest absolute quantum yield, reaching 20.25% and 4.81%, respectively.

Silicate-clad Dy3+ doped multi-component phosphate glass core glass fiber for yellow laser applications

In this work, strong yellow emission was obtained in Dy3+ doped multi-component phosphate glass due to its high asymmetry and covalency of the local field and high phonon energy. The internal quantum efficiency was measured to be 39.27% and the figure of merit was calculated to be 210.53 pm2 × μs. What is more, silicate-clad Dy3+ doped multi-component phosphate core glass fiber was successfully drawn by using a rod-in-tube method, which has a strong fluorescence emission in yellow spectra band. The Dy3+ doping concentration is 2.6 wt.%, which is much larger than that of Dy3+ doped (0.2 wt.%) ZBLAN fiber. These results suggest that the silicate-clad Dy3+ doped multi-component phosphate glass fibers are potential host matrices for yellow laser.

Utilization of GelMA with phosphate glass fibers for glial cell alignment.

Glial cell alignment in tissue engineered constructs is essential for achieving functional outcomes in neural recovery. While gelatin methacrylate (GelMA) hydrogel offers superior biocompatibility along with permissive structure and tailorable mechanical properties, phosphate glass fibers (PGFs) can provide physical cues for directionality of neural growth. Aligned PGFs were fabricated by a melt quenching and fiber drawing method and utilized with synthesized GelMA hydrogel. The mechanical properties of GelMA and biocompatibility of the GelMA-PGFs composite were investigated in vitro using rat glial cells. GelMA with 86% methacrylation degree were photo-crosslinked using 0.1%wt photo-initiator (PI). Photocrosslinking under UV exposure for 60 s was used to produce hydrogels (GelMA-60). PGFs were introduced into the GelMA before crosslinking. Storage modulus and loss modulus of GelMA-60 was 24.73 ± 2.52 and 1.08 ± 0.23 kN/m2 , respectively. Increased cell alignment was observed in GelMA-PGFs compared with GelMA hydrogel alone. These findings suggest GelMA-PGFs can provide glial cells with physical cues necessary to achieve cell alignment. This approach could further be used to achieve glial cell alignment in bioengineered constructs designed to bridge damaged nerve tissue.

Additive-Manufactured Gyroid Scaffolds of Magnesium Oxide, Phosphate Glass Fiber and Polylactic Acid Composite for Bone Tissue Engineering.

Composites of biodegradable phosphate glass fiber and polylactic acid (PGF/PLA) show potential for bone tissue engineering scaffolds, due to their ability to release Ca, P, and Mg during degradation, thus promoting the bone repair. Nevertheless, glass degradation tends to acidify the surrounding aqueous environment, which may adversely affect the viability and bone-forming activities of osteoblasts. In this work, MgO was investigated as a neutralizing agent. Porous network-phase gyroid scaffolds were additive-manufactured using four different materials: PLA, MgO/PLA, PGF/PLA, and (MgO + PGF)/PLA. The addition of PGF enhanced compressive properties of scaffolds, and the resultant scaffolds were comparably strong and stiff with human trabecular bone. While the degradation of PGF/PLA composite induced considerable acidity in degradation media and intensified the degradation of PGF in return, the degradation media of (MgO + PGF)/PLA maintained a neutral pH close to a physiological environment. The experiment results indicated the possible mechanism of MgO as the neutralizing agent: the local acidity was buffered as the MgO reacted with the acidic degradation products thereby inhibiting the degradation of PGF from being intensified in an acidic environment. The (MgO + PGF)/PLA composite scaffold appears to be a candidate for bone tissue engineering.

An Eye-Safe, SBS-Free Coherent Fiber Laser LIDAR Transmitter with Millijoule Energy and High Average Power

We report on an eye-safe, transform-limited, millijoule energy, and high average power fiber laser. The high gain and short length of the NP phosphate-glass fibers enable the SBS-free operation with kW level peak power. The output energy is up to 1.3 mJ, and the average power is up to 23 W at an 18 kHz repetition rate with 600 ns pulses (peak power > 2.1 kW). The PER is ≈16 dB and the M2 of the beam is 1.33 × 1.18. The coherent LIDAR Figure Of Merit (FOM) is 174 mJ*sqrt(Hz), which to our knowledge is the highest reported for a fiber laser. We also report 0.75 mJ energy and >3.7 kW peak power with down to 200 ns pulses and up to 1.21 mJ energy with a 3–5 kHz repetition rate operation of the current system.

Single-Frequency Nd3+-Doped Phosphate Fiber Laser at 915 nm

Single-frequency distributed Bragg reflector fiber laser at 915 nm was demonstrated by using a 2.5-cm long Nd3+-doped phosphate fiber as the gain medium. An output power of 13.5 mW was obtained at an absorbed pump power of 240 mW. Our experimental results show that Nd3+-doped phosphate glass fiber is more efficient than Nd3+-doped silica glass fiber for single-frequency laser operation in the 900 nm wavelength range.