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Keywords = Si–glass bonding

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32 pages, 6710 KiB  
Article
XPS Investigation of Sol–Gel Bioactive Glass Synthesized with Geothermal Water
by Helena Cristina Vasconcelos, Maria Meirelles and Reşit Özmenteş
Surfaces 2025, 8(3), 50; https://doi.org/10.3390/surfaces8030050 - 14 Jul 2025
Viewed by 197
Abstract
Bioactive glasses are known for their surface reactivity and ability to bond with bone tissue through the formation of hydroxyapatite. This study investigates the effects of substituting ultrapure water with natural geothermal waters from the Azores in the sol–gel synthesis of 45S5 and [...] Read more.
Bioactive glasses are known for their surface reactivity and ability to bond with bone tissue through the formation of hydroxyapatite. This study investigates the effects of substituting ultrapure water with natural geothermal waters from the Azores in the sol–gel synthesis of 45S5 and MgO-modified bioglasses. Using high-resolution X-ray photoelectron spectroscopy (XPS), we examined how the mineral composition of the waters influenced the chemical environment and network connectivity of the glass surface. The presence of trace ions, such as Mg2+, Sr2+, Zn2+, and B3+, altered the silicate structure, as evidenced by binding energy shifts and peak deconvolution in O 1s, Si 2p, P 2p, Ca 2p, and Na 1s spectra. Thermal treatment further promoted polymerization and reduced hydroxylation. Our findings suggest that mineral-rich waters act as functional agents, modulating the reactivity and structure of bioactive glass surfaces in eco-sustainable synthesis routes. Full article
(This article belongs to the Special Issue Bio-Inspired Surfaces)
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13 pages, 2079 KiB  
Article
Preparation and Properties of a Composite Glass Protective Lubricating Coating for the Forging of Ti-6Al-4V Alloy
by Zunqi Xiao, Qiuyue Xie, Bin Zhang, Bing Ren and Shujian Tian
Coatings 2025, 15(7), 792; https://doi.org/10.3390/coatings15070792 - 5 Jul 2025
Viewed by 359
Abstract
A SiO2-Al2O3-B2O3-CaO-MgO-Na2O glass-based protective lubricant coating was developed for Ti-6Al-4V alloy forging, featuring a fully non-toxic formulation. The coating consisted of a composite glass matrix formed by blending two phases with [...] Read more.
A SiO2-Al2O3-B2O3-CaO-MgO-Na2O glass-based protective lubricant coating was developed for Ti-6Al-4V alloy forging, featuring a fully non-toxic formulation. The coating consisted of a composite glass matrix formed by blending two phases with distinct softening temperatures, extending its operational window to 700–950 °C. The composite glass showed initial softening at 700 °C and complete melting at 800 °C, with contact angle measurements confirming superior wettability (θ < 90°) across the forging range (800~950 °C). With an increase in temperature, the surface tension of the composite glass melt decreased, and subsequently, the wettability of the composite glass melt was significantly improved. XRD revealed that the uncoated Ti-6Al-4V formed a 22 μm thick rutile TiO2 scale with a porous structure and interfacial cracks, while the coated sample retained an amorphous glass layer with no TiO2. Cross-sectional SEM showed a crack-free, poreless interface with strong metallurgical bonding, in contrast to the uncoated sample’s spalled oxide layer. EDS showed minimal oxygen diffusion of the glass coating into the substrate. Ring upsetting tests showed that the coating reduced friction from 0.5–0.7 to 0.3 (50–57% decrease). Collectively, the glass protective lubricant coating showed good performance in terms of protection and lubrication. Full article
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28 pages, 11703 KiB  
Article
Enhancing the Interfacial Adhesion and Mechanical Strength of Pultruded ECR–Glass Fiber Composites with Nanofiller-Infused Epoxy Resin
by Poorna Chandra, Ravikumar Venkatarayappa, Savitha D. Chandrashekar, Kiran Raveendra, Asha P. Bhaskararao, Suresha Bheemappa, Dayanand M. Goudar, Rajashekhar V. Kurhatti, K. Raju and Deesy G. Pinto
J. Compos. Sci. 2025, 9(7), 321; https://doi.org/10.3390/jcs9070321 - 23 Jun 2025
Viewed by 895
Abstract
The effect of the interaction between silica (nS) and hydroxyapatite (nHap) nanomaterials on the characteristics of unidirectional glass-fiber-reinforced epoxy (GF/Ep) composite systems is investigated in this work. The goal of the study is to use these nanofillers to improve the microstructure and mechanical [...] Read more.
The effect of the interaction between silica (nS) and hydroxyapatite (nHap) nanomaterials on the characteristics of unidirectional glass-fiber-reinforced epoxy (GF/Ep) composite systems is investigated in this work. The goal of the study is to use these nanofillers to improve the microstructure and mechanical characteristics. Pultrusion was used to produce hybrid nanocomposites while keeping the GF loading at a consistent 75% by weight. The hybrid nanocomposites were made with a total filler loading of 6 wt.%, including nHap, and a nS loading ranging from 2 to 4 wt.%. The mechanical performance of the composite was greatly improved by the use of these nanofillers. Compared to neat GF/Ep, hybrid nanocomposites with 6 wt.% combined fillers exhibited increased hardness (14%), tensile strength (25%), interlaminar shear strength (21.3%), and flexural strength (33%). These improvements are attributed to efficient filler dispersion, enhanced fiber-matrix adhesion, and crack propagation resistance. Incorporating 4 wt.% nS alone improved hardness (6%), tensile strength (9%), tensile modulus (21%), interlaminar shear strength (11.4%), flexural strength (12%), and flexural modulus (14%). FTIR analysis indicated Si-O-Si network formation and increased hydrogen bonding, supporting enhanced interfacial interactions. Ultraviolet reflectance measurements showed increased UV reflectivity with nS, especially in hybrid systems, due to synergistic effects. Impact strength also improved, with a notable 11.6% increase observed in the hybrid nanocomposite. Scanning and transmission electron microscopy confirmed that the nanofillers act as secondary reinforcements within the matrix. These hybrid nanocomposites present a promising material choice for various industries, including marine structural applications and automotive components. Full article
(This article belongs to the Special Issue Mechanical Properties of Composite Materials and Joints)
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24 pages, 7602 KiB  
Article
Developing Bioengineered 3D-Printed Composite Scaffolds with Antimicrobial Potential for Bone Tissue Regeneration
by Andreea Trifan, Eduard Liciu, Cristina Busuioc, Izabela-Cristina Stancu, Adela Banciu, Carmen Nicolae, Mihai Dragomir, Doru-Daniel Cristea, Rosina-Elena Sabău, David-Andrei Nițulescu and Alexandru Paraschiv
J. Funct. Biomater. 2025, 16(6), 227; https://doi.org/10.3390/jfb16060227 - 19 Jun 2025
Viewed by 787
Abstract
This research activity proposes to produce composite hydrogel–bioactive glass. The primary purpose of this research is to develop and optimize 3D-printed scaffolds using doped bioglass, aimed at enhancing bone regeneration in bone defects. The bioglass, a bioactive material known for its bone-bonding ability [...] Read more.
This research activity proposes to produce composite hydrogel–bioactive glass. The primary purpose of this research is to develop and optimize 3D-printed scaffolds using doped bioglass, aimed at enhancing bone regeneration in bone defects. The bioglass, a bioactive material known for its bone-bonding ability (SiO2–P2O5–CaO–Na2O), co-doped with europium and silver was synthesized and doped to improve its biological properties. This doped bioglass was then combined with a biocompatible hydrogel, chosen for its adequate cellular response and printability. The composite material was printed to form a scaffold, providing a structure that not only supports the damaged bone but also encourages osteogenesis. A variety of methods were employed to assess the rheological, compositional, and morphological characteristics of the samples: Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). Additionally, simulated body fluid (SBF) immersion for bioactivity monitoring and immunocytochemistry for cell viability were used to evaluate the biological response of the scaffolds. Full article
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15 pages, 3887 KiB  
Article
Cold Consolidation of Waste Glass by Alkali Activation and Curing by Traditional and Microwave Heating
by Francesco Carollo, Emanuele De Rienzo, Antonio D’Angelo, Paolo Sgarbossa, Luisa Barbieri, Cristina Leonelli, Isabella Lancellotti, Michelina Catauro and Enrico Bernardo
Materials 2025, 18(11), 2628; https://doi.org/10.3390/ma18112628 - 4 Jun 2025
Viewed by 575
Abstract
Despite efforts to recycle, boro-alumino-silicate pharmaceutical glass (BASG) results in a significant portion of glass cullet currently landfilled. Highly contaminated fractions of BASG cullet are largely unemployed because of the presence of metals in their composition that prevents recycling. This waste glass can [...] Read more.
Despite efforts to recycle, boro-alumino-silicate pharmaceutical glass (BASG) results in a significant portion of glass cullet currently landfilled. Highly contaminated fractions of BASG cullet are largely unemployed because of the presence of metals in their composition that prevents recycling. This waste glass can be eligible to produce sustainable alkali-activated materials (AAMs) reducing at the same time consumption of raw materials and CO2 emissions. The ‘weak’ alkaline attack (NaOH < 3 M) determines the gelation of glass suspensions. Condensation reactions occur in hydrated surface layers, leading to strong bonds (Si-O-Si, Al-O-Si, etc.) between individual glass particles. Alkali are mostly expelled from the gel due to the formation of water-soluble hydrated carbonates. Microwave treatment has been implemented on samples after precuring at 40 °C, saving time and energy and achieving better mechanical properties. To improve the stability and reduce the release of glass components into solution, the consolidated monoliths were subjected to boiling/drying cycles. The chemical stability, cytotoxicity and antibacterial behavior of the final products have been investigated with the purpose of obtaining new competitive and sustainable materials. For further stabilization and for finding new applications, the activated and boiled samples can be fired at low temperature (700 °C) to obtain, respectively, a homogeneous foam or a compact material with glass-like density and microstructure. Full article
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15 pages, 2302 KiB  
Article
Experimental Investigation and Molecular Dynamics Modeling of the Effects of K2O on the Structure and Viscosity of SiO2-CaO-Al2O3-MgO-K2O Slags at High Temperatures
by Fan Yang, Qingguo Xue, Haibin Zuo, Yu Liu and Jingsong Wang
Metals 2025, 15(6), 590; https://doi.org/10.3390/met15060590 - 25 May 2025
Viewed by 431
Abstract
Variations in slag properties critically influence smelting operations and product quality. The effects of K2O on the CaO-SiO2-MgO-Al2O3-K2O slag system at 1823 K were systematically analyzed through an integrated approach combining viscosity measurements, [...] Read more.
Variations in slag properties critically influence smelting operations and product quality. The effects of K2O on the CaO-SiO2-MgO-Al2O3-K2O slag system at 1823 K were systematically analyzed through an integrated approach combining viscosity measurements, FTIR spectroscopy, and molecular dynamics simulations. The results revealed a rapid 52% decrease in slag viscosity and an 18.32 kJ/mol reduction in activation energy as K2O content increased from 0% to 3%. K2O releases O2− ions that depolymerize Si-O network structures. Within the 3% to 5% range, structural network formation is promoted by the K2O-SiO2 reaction, resulting in increased slag viscosity and elevated activation energy. Molecular dynamics simulations elucidate the depolymerization of complex Si-O networks, accompanied by a proliferation of smaller [AlO4] tetrahedral fragments. The diminished Si-O-Si bridging oxygen (BO) bonds contrast with the enhanced increase in Si-O-K non-bridging oxygen (NBO) linkages. When K2O exceeds 3%, the diffusion capacity of K atoms becomes constrained as K2O participates in structural network assembly, a phenomenon validated by FTIR spectroscopic analysis. Elevated K2O concentrations enhance slag network polymerization, leading to increased viscosity. Therefore, the precise control of K2O content is critical during smelting operations and by-product manufacturing (e.g., glass or mineral wool) to optimize material performance. These findings provide theoretical support for controlling the alkali metal content during the actual metallurgical process and thus further optimizing blast furnace operation. Full article
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24 pages, 4250 KiB  
Article
Interactions and Curing Dynamics Between UV-Triggered Epoxy Acrylate Binder, Curing Agents and Photoinitiators
by Ji-min Choi, Sang Jang and Keon-Soo Jang
Polymers 2025, 17(9), 1252; https://doi.org/10.3390/polym17091252 - 4 May 2025
Viewed by 852
Abstract
This study investigated the interaction between UV-triggered curing binders and photoinitiators, focusing on their thermal, mechanical, and morphological properties. Using epoxy acrylate as the matrix and three potential photoinitiators with varying phosphorus contents, UV curing systems were fabricated and analyzed. 2-hydroxy-2-methyl-1-phenyl-1-propanone (HMPP), 2,4,6-trimethyl [...] Read more.
This study investigated the interaction between UV-triggered curing binders and photoinitiators, focusing on their thermal, mechanical, and morphological properties. Using epoxy acrylate as the matrix and three potential photoinitiators with varying phosphorus contents, UV curing systems were fabricated and analyzed. 2-hydroxy-2-methyl-1-phenyl-1-propanone (HMPP), 2,4,6-trimethyl benzoyl diphenyl phosphine oxide (TPO), and their mixture were utilized as photoinitiators. We observed that the curing process significantly reduced residual double bonds within the first 5 s of UV irradiation time. The glass transition temperature (Tg) increased with curing time due to enhanced network density. For instance, in the MyA–TPO formulation, Tg of the cured sample tended to increase to 67.3 °C for 3 s to 79.8 °C for 15 s. Mechanical analysis revealed that HMPP facilitated the formation of robust network structures. Notably, the MyA–HMPP formulation exhibited a tensile strength of 63 MPa and a Young’s modulus of 21 MPa, indicating excellent mechanical strength. SEM imaging confirmed these findings, illustrating distinct fracture morphologies that correlated with mechanical performance. These results provide insights into optimizing UV-curable materials for applications requiring high precision and durability. In particular, the combination of high Tg, superior tensile strength, and uniform fracture morphology indicates excellent thermal stability, mechanical integrity, and crack resistance—critical requirements in semiconductor packaging. These properties, along with rapid UV curing, support the suitability of the proposed systems for advanced applications such as system-in-package (SiP) and 3D integration. Full article
(This article belongs to the Special Issue Advanced Epoxy-Based Materials, 5th Edition)
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22 pages, 2515 KiB  
Review
A Review of Joining Technologies for SiC Matrix Composites
by Yongheng Lu, Jinzhuo Zhang, Guoquan Li, Zaihong Wang, Jing Wu and Chong Wei
Materials 2025, 18(9), 2046; https://doi.org/10.3390/ma18092046 - 30 Apr 2025
Viewed by 759
Abstract
SiC matrix composites are widely used in high-temperature structural components of aircraft engines and nuclear reactor materials because of their excellent properties such as their high modulus, high strength, corrosion resistance, and high-temperature resistance. However, the bonding of SiCf/SiC composites poses significant challenges [...] Read more.
SiC matrix composites are widely used in high-temperature structural components of aircraft engines and nuclear reactor materials because of their excellent properties such as their high modulus, high strength, corrosion resistance, and high-temperature resistance. However, the bonding of SiCf/SiC composites poses significant challenges in practical engineering applications, primarily due to residual stresses, anisotropy in composite properties, and the demanding conditions required for high-performance joints. This work reviews various bonding technologies for SiC ceramics and SiC matrix composites. These include solid-state diffusion bonding, NITE phase bonding, direct bonding without filling materials, MAX phase bonding, glass ceramic bonding, polymer precursor bonding, metal brazing bonding, and Si-C reaction bonding. Key results, such as the highest bending strength of 439 MPa achieved with Si-C reaction bonding, are compared alongside the microstructural characteristics of different joints. Additionally, critical factors for successful bonding, such as physical mismatch and metallurgical incompatibility, are discussed in detail. Future research directions are proposed, emphasizing the optimization of bonding techniques and evaluation of joint performance in harsh environments. This review provides valuable insights into advancing bonding technologies for SiC composites in aerospace and nuclear applications. Full article
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15 pages, 6891 KiB  
Article
Reactions of Hydrogen-Passivated Silicon Vacancies in α-Quartz with Electron Holes and Hydrogen
by Teofilo Cobos Freire, Jack Strand and Alexander L. Shluger
Nanomaterials 2025, 15(2), 142; https://doi.org/10.3390/nano15020142 - 19 Jan 2025
Viewed by 1037
Abstract
We used density functional theory with a hybrid functional to investigate the structure and properties of [4H]Si (hydrogarnet) defects in α-quartz as well as the reactions of these defects with electron holes and extra hydrogen atoms and ions. The results demonstrate [...] Read more.
We used density functional theory with a hybrid functional to investigate the structure and properties of [4H]Si (hydrogarnet) defects in α-quartz as well as the reactions of these defects with electron holes and extra hydrogen atoms and ions. The results demonstrate the depassivation mechanisms of hydrogen-passivated silicon vacancies in α-quartz, providing a detailed understanding of their stability, electronic properties, and behaviour in different charge states. While fully hydrogen passivated silicon vacancies are electrically inert, the partial removal of hydrogen atoms activates these defects as hole traps, altering the defect states and influencing the electronic properties of the material. Our calculations of the hydrogen migration mechanisms predict the low energy barriers for H+, H0, and H, with the lowest barrier of 0.28 eV for neutral hydrogen migration between parallel c-channels and a similar barrier for H+ migration along the c-channels. The reactions of electron holes and hydrogen species with [4H]Si defects lead to the breaking of O–H bonds and the formation of non-bridging oxygen hole centres (NBOHCs) within the Si vacancies. The calculated optical absorption energies of these centres are close to those attributed to individual NBOHCs in glass samples. These findings can be useful for understanding the role of [4H]Si defects in bulk and nanocrystalline quartz as well as in SiO2-based electronic devices. Full article
(This article belongs to the Section Theory and Simulation of Nanostructures)
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15 pages, 4481 KiB  
Article
Characterization of Grape Extract-Colored SiO2 Synthesized via the Sol–Gel Method
by Marika Fiorentino, Antonio D’Angelo, Luigi Vertuccio, Humaira Khan and Michelina Catauro
Appl. Sci. 2024, 14(24), 11697; https://doi.org/10.3390/app142411697 - 15 Dec 2024
Viewed by 1018
Abstract
Numerous studies have focused on the development of active packaging using plastics, but glass-based active packaging represents a more sustainable alternative, offering advantages in terms of recyclability, durability, and reduced environmental footprint. This study proposes a glass-based active packaging system by incorporating anthocyanins-rich [...] Read more.
Numerous studies have focused on the development of active packaging using plastics, but glass-based active packaging represents a more sustainable alternative, offering advantages in terms of recyclability, durability, and reduced environmental footprint. This study proposes a glass-based active packaging system by incorporating anthocyanins-rich grape extract (GRE) into a silica (SiO2) matrix using the sol–gel method. GRE was added at two concentrations, 5% (S5GRE) and 15% (S15GRE). During synthesis, color brightening occurred as anthocyanins shifted to colorless chalcone and pseudo-base forms, but colorimetric analysis confirmed that the hybrid materials retained a red hue after gel drying. Fourier-transform infrared (FTIR) and thermogravimetric analysis (TGA/DTG) investigated the stability of the GRE within the silica matrix and showed that both hybrids formed hydrogen bonds with the inorganic matrix. However, S5GRE exhibited better thermal stability compared to that of S15GRE, possibly due to a greater proportion of the extract being fully entrapped rather than surface-bound. The encapsulation efficiency analysis supported this, showing that 98.12% of the GRE was successfully entrapped in S5GRE, whereas S15GRE retained only 54.62%. These results indicate that, while S5GRE exhibits higher encapsulation efficiency and allows for faster release, S15GRE releases less efficiently due to extract aggregation within the matrix. Full article
(This article belongs to the Section Chemical and Molecular Sciences)
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22 pages, 8070 KiB  
Article
Structure, Optical and Electrical Properties of Nb(Zn) Doped Sol–Gel ITO Films: Effect of Substrates and Dopants
by Mariuca Gartner, Anna Szekeres, Simeon Simeonov, Maria Covei, Mihai Anastasescu, Silviu Preda, Jose Maria Calderon-Moreno, Luminita Predoana, Hermine Stroescu, Daiana Mitrea and Madalina Nicolescu
Molecules 2024, 29(22), 5480; https://doi.org/10.3390/molecules29225480 - 20 Nov 2024
Viewed by 1062
Abstract
We present comparative studies of sol–gel ITO multilayered films undoped and doped with Nb or Zn (4 at.%). The films were obtained by successive depositions of five layers using the dip-coating sol–gel method on microscopic glass, SiO2/glass, and Si substrates. The [...] Read more.
We present comparative studies of sol–gel ITO multilayered films undoped and doped with Nb or Zn (4 at.%). The films were obtained by successive depositions of five layers using the dip-coating sol–gel method on microscopic glass, SiO2/glass, and Si substrates. The influence of the type of substrates and dopant atoms on the structure and optical properties of the sol–gel ITO thin films is examined and discussed in detail. XRD patterns of these layers showed a polycrystalline structure with an average crystallite size of <11 nm. Raman spectroscopy confirmed the chemical bonding of dopants with oxygen and showed the absence of crystallized Nb(Zn)-oxide particles, indicated by the XRD pattern. Spectroscopic Ellipsometry and AFM imaging revealed a clear dependence of the optical parameters and surface morphology of the ITO and ITO:Nb(Zn) thin films on the type of substrates and dopants. The analysis of the current-voltage and capacitance-voltage characteristics of the Al/ITO/Si structures revealed the presence of charge carrier traps in the ITO bulk and the ITO-Si interface. The densities of these traps are obtained and the character of the current transport mechanism is established. Full article
(This article belongs to the Special Issue Chemical Research on High-Performance Composites)
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14 pages, 7530 KiB  
Article
Cold Consolidation of Pharmaceutical Waste Glass Powders Through Alkali Activation and Binder Jet 3D Printing
by Hamada Elsayed, Filippo Gobbin, Alberto Barci, Enrico Bernardo and Paolo Colombo
Materials 2024, 17(21), 5164; https://doi.org/10.3390/ma17215164 - 23 Oct 2024
Cited by 2 | Viewed by 1247
Abstract
The recent COVID-19 emergency has led to an impressive increase in the production of pharmaceutical vials. This has led to a parallel increase in the amounts of waste glass; manufacturers typically recover material from faulty containers by crushing, giving origin to an unrecyclable [...] Read more.
The recent COVID-19 emergency has led to an impressive increase in the production of pharmaceutical vials. This has led to a parallel increase in the amounts of waste glass; manufacturers typically recover material from faulty containers by crushing, giving origin to an unrecyclable fraction. Coarse fragments are effectively reused as feedstock for glass melting; on the contrary, fine powders (<100 microns), contaminated by metal and ceramic particles due to the same crushing operations, are landfilled. Landfilling is also suggested for pharmaceutical containers after medical use. This study aims at proposing new opportunities for the recycling of fine glass particles, according to recent findings concerning alkali activation of pharmaceutical glass, combined with novel processing, i.e., binder jetting printing. It has already been shown that pharmaceutical glass, immersed in low-molarity alkaline solution (not exceeding 2.5 M NaOH), undergoes surface dissolution and hydration; cold consolidation is later achieved, upon drying at 40–60 °C, by a condensation reaction occurring at hydrated layers of adjacent particles. Binder jetting printing does not realize a full liquid immersion of the glass powders, as the attacking solution is selectively sprayed on a powder bed. Here, we discuss the tuning of key parameters, such as the molarity of the attacking solution (from 2.5 to 10 M) and the granulometry of the waste glass, to obtain stable printed blocks. In particular, the stability depends on the formation of bridges between adjacent particles consisting of strong T-O bonds (Si-O-Si, Al-O-Si, B-O-Si), while degradation products (concentrating Na ions) remain as a secondary phase, solubilized by immersion in boiling water. Such stability is achieved by operating at 5 M NaOH. Full article
(This article belongs to the Special Issue State of the Art of Materials Science and Engineering in Italy)
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20 pages, 3103 KiB  
Article
Polymers Containing Diethylsiloxane Segment and Active Functional Group by Ring-Opening Polymerization of Hexaethylcyclotrisiloxane under the Catalysis of Linear Chlorinated Phosphazene Acid
by Chen Jin, Hao Yang, Yang Zhang, Shuting Zhang, Xu Long, Hong Dong, Yanjiang Song, Zhirong Qu and Chuan Wu
Polymers 2024, 16(19), 2835; https://doi.org/10.3390/polym16192835 - 7 Oct 2024
Cited by 1 | Viewed by 1640
Abstract
Linear chlorinated phosphazene acid is prepared using PCl5 and NH4Cl as raw materials. Using hexaethylcyclotrisiloxane as the monomer, 1,1,3,3-tetramethyldisiloxane or 1,3-divinyl-1,1,3,3-tetramethyldisiloxane as the end-capping agent, and linear chlorinated phosphazene acid as the catalyst, polydiethylsiloxane oligomers terminated with active Si-H or [...] Read more.
Linear chlorinated phosphazene acid is prepared using PCl5 and NH4Cl as raw materials. Using hexaethylcyclotrisiloxane as the monomer, 1,1,3,3-tetramethyldisiloxane or 1,3-divinyl-1,1,3,3-tetramethyldisiloxane as the end-capping agent, and linear chlorinated phosphazene acid as the catalyst, polydiethylsiloxane oligomers terminated with active Si-H or Si-CH=CH2 groups have been prepared. Using hexaethylcyclotrisiloxane and 1,3,5,7-octamethylcyclotetrasiloxane as comonomers, 1,1,3,3-tetramethyldisiloxane or hexamethyldisiloxane as the end-capping agent, or using hexaethylcyclotrisiloxane and octamethylcyclotetrasiloxane as comonomers, 1,1,3,3-tetramethyldisiloxane as the end-capping agent, copolymers containing active Si-H bonds and dimethylsiloxane segments have been prepared under the catalysis of linear chlorinated phosphazene acid. The effects of catalyst dosage, reaction temperature, reaction time, end-capping agent, and polymerization monomer dosage on polymer yield and structure were investigated. Using 300 ppm of linear chlorinated phosphazene acid, oligomers and copolymers containing an active Si-H bond and diethylsiloxane segment were prepared under mild conditions. The molecular weight of the obtained polymers was close to their designed values, but their PDI values were small. The highest yield of α, ω-bisdimethylsiloxyl-terminated PDES oligomers reached 93%. Using oligomers and copolymers containing Si-H bonds and diethylsiloxane segments as crosslinkers, a silicone gel containing diethylsiloxane segments was prepared by hydrosilylation reaction. With the introduction of a diethylsiloxane segment, the glass transition temperature of the silicone gel decreased relative to that of the PDMS oligomer, but the temperature at 5% weight loss in nitrogen atmosphere decreased from 347 °C to 312 °C. The mechanism of the ring-opening polymerization of hexaethylcyclotrisiloxane catalyzed by linear chlorinated phosphazene acid is also discussed. Full article
(This article belongs to the Section Polymer Chemistry)
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25 pages, 3993 KiB  
Article
Structural and Dynamical Effects of the CaO/SrO Substitution in Bioactive Glasses
by Margit Fabian, Matthew Krzystyniak, Atul Khanna and Zsolt Kovacs
Molecules 2024, 29(19), 4720; https://doi.org/10.3390/molecules29194720 - 5 Oct 2024
Viewed by 1437
Abstract
Silicate glasses containing silicon, sodium, phosphorous, and calcium have the ability to promote bone regeneration and biodegrade as new tissue is generated. Recently, it has been suggested that adding SrO can benefit tissue growth and silicate glass dissolution. Motivated by these recent developments, [...] Read more.
Silicate glasses containing silicon, sodium, phosphorous, and calcium have the ability to promote bone regeneration and biodegrade as new tissue is generated. Recently, it has been suggested that adding SrO can benefit tissue growth and silicate glass dissolution. Motivated by these recent developments, the effect of SrO/CaO–CaO/SrO substitution on the local structure and dynamics of Si-Na-P-Ca-O oxide glasses has been studied in this work. Differential thermal analysis has been performed to determine the thermal stability of the glasses after the addition of strontium. The local structure has been studied by neutron diffraction augmented by Reverse Monte Carlo simulation, and the local dynamics by neutron Compton scattering and Raman spectroscopy. Differential thermal analysis has shown that SrO-containing glasses have lower glass transition, melting, and crystallisation temperatures. Moreover, the addition of the Sr2+ ions decreased the thermal stability of the glass structure. The total neutron diffraction augmented by the RMC simulation revealed that Sr played a similar role as Ca in the glass structure when substituted on a molar basis. The bond length and the coordination number distributions of the network modifiers and network formers did not change when SrO (x = 0.125, 0.25) was substituted for CaO (25-x). However, the network connectivity increased in glass with 12.5 mol% CaO due to the increased length of the Si-O-Si interconnected chain. The analysis of Raman spectra revealed that substituting CaO with SrO in the glass structure dramatically enhances the intensity of the high-frequency band of 1110–2000 cm−1. For all glasses under investigation, the changes in the relative intensities of Raman bands and the distributions of the bond lengths and coordination numbers upon the SrO substitution were correlated with the values of the widths of nuclear momentum distributions of Si, Na, P, Ca, O, and Sr. The widths of nuclear momentum distributions were observed to soften compared to the values observed and simulated in their parent metal-oxide crystals. The widths of nuclear momentum distributions, obtained from fitting the experimental data to neutron Compton spectra, were related to the amount of disorder of effective force constants acting on individual atomic species in the glasses. Full article
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10 pages, 2393 KiB  
Article
The Effects of Different Blending Methods on the Thermal, Mechanical, and Optical Properties of PMMA/SiO2 Composites
by Chi-Kai Lin, Jia-Wei Xie, Ping-Jui Tsai, Hao-Yu Wang, Zhi-Wei Lu, Tung-Yi Lin and Chih-Yu Kuo
J. Compos. Sci. 2024, 8(9), 369; https://doi.org/10.3390/jcs8090369 - 20 Sep 2024
Cited by 2 | Viewed by 1764
Abstract
In this study, PMMA/SiO2 composites were fabricated with monodispersed SiO2 and PMMA using four distinct methods—physical blending, in situ polymerization, random copolymerization, and block copolymerization—to investigate the composites’ thermal, mechanical, and optical properties. In the physical blending approach, SiO2 nanoparticles [...] Read more.
In this study, PMMA/SiO2 composites were fabricated with monodispersed SiO2 and PMMA using four distinct methods—physical blending, in situ polymerization, random copolymerization, and block copolymerization—to investigate the composites’ thermal, mechanical, and optical properties. In the physical blending approach, SiO2 nanoparticles were dispersed in a PMMA solution, while during in situ polymerization, silica nanoparticles were incorporated during the synthesis of PMMA/SiO2 composites. 3-methacryloxypropyltrimethoxysilane (MPS) was modified on the SiO2 surface to introduce the reactive double bonds. The MPS@SiO2 was either random- or block-copolymerized with PMMA through RAFT polymerization. The PMMA/SiO2 composites prepared via these different methods were characterized using FTIR, TGA, and DSC to determine their chemical structures, thermal degradation temperatures, and glass transition temperatures, respectively. Scanning electron microscopy (SEM) was employed to observe the microstructures and dispersion of the composites. This comprehensive analysis revealed that the PMMA/SiO2 composites prepared via block copolymerization exhibited thermal stability at temperatures between 200 and 300 °C. Additionally, they demonstrated excellent transparency (86%) and scratch resistance (≥6H) while maintaining mechanical strength, suggesting their potential application in thermal insulation materials. Full article
(This article belongs to the Special Issue Progress in Polymer Composites, Volume III)
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