Fire-Resistant and Thermal Stability Properties of Fluorosilicone Adhesives by Incorporation of Surface-Modified Aluminum Trihydrate.

Fluorosilicone was combined with aluminum trihydrate (ATH) to induce synergistic flame-retardant and thermal-resistant properties. The surface of ATH was modified with four different silane coupling agents. The flammability and mechanical properties of the fluorosilicone/ATH composites were assessed using an UL94 vertical test and a die shear strength test. The change in shear strength was investigated under aging for 1000 h at -55 °C and 150 °C. Pure fluorosilicone had inherent fire resistance and thus achieved a V-0 rating even at 20 wt.% ATH loading. Upon addition of ATH treated with 3-glycidoxypropyl trimethoxysilane, the composites exhibited the highest shear strength of 3.9 MPa at 23 °C because of the additional crosslinking reaction of fluorosilicone resin with the epoxide functional group of the coupling agent. Regardless of the types of coupling agents, the composites exhibited similar flame retardancy at the same ATH content, with a slight reduction in shear strength at 180 °C and 250 °C. The shear strength of the adhesives gradually decreased with aging time at -55 °C, but increased noticeably from 3.9 MPa to 11.5 MPa when aged at 150 °C due to the occurrence of the additional crosslinking reaction of fluorosilicone.

Adhesion Strength Enhancement of Butyl Rubber and Aluminum Using Nanoscale Self-Assembled Monolayers of Various Silane Coupling Agents for Vibration Damping Plates.

In this paper, we enhance the adhesion strength of butyl rubber-based vibrational damping plates using nanoscale self-assembled monolayers of various silane coupling agents. The silane coupling agents used to chemically modify the plate's aluminum surface include 3-aminopropyltriethoxysilane (APTES), (3-glycidyloxypropyl) triethoxysilane (GPTES), 3-mercaptopropyltrimethoxysilane (MPTMS), and 3-(triethoxysilyl)propyl isocyanate (ICPTES). The modified surfaces were analyzed using Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the enhancement in adhesion strength between the rubber and aluminum was estimated through T-Peel tests. As a result, MPTMS showed the highest enhancement in adhesion strength, of approximately 220% compared to the untreated sample, while GPTES, ICPTES, and APTES resulted in adhesion strength enhancements of approximately 200%, 150%, and 130%, respectively.

Effect of the surface coating of carbonyl iron particles on the dispersion stability of magnetorheological fluid.

The dispersion stability of carbonyl iron particle (CIP)-based magnetorheological fluid (MRF) is improved by CIP, which particle is etched with hydrochloric acid (HCl) to form porous structure with many hydroxyl groups and subsequently coated with silane coupling agents that have varying chain lengths. The microstructures, coating effect and magnetism of the CIPs were examined using the Scanning Electron Microscopy, Automatic Surface and Porosity Analyzer (BET), Fourier-Transform Infrared Spectroscopy, Thermogravimetric Analysis and Vibrating Sample Magnetometer. Furthermore, the rheological properties and dispersion stability of the MRFs were assessed using a Rotating Rheometer and Turbiscan-lab. The results revealed that the nanoporous structure appeared on the CIPs and the specific surface area increased remarkably after being etched by hydrochloric acid. Additionally, as the chain length of the silane coupling agent increases, the coated mass on the particles increases, the the density and the saturation magnetization of particles decreased, and the coated particles with different shell thicknesses were obtained; without a magnetic field, the viscosity of MRF prepared by coated particles increase slightly, due to the enhancement of special three-dimensional network structure; under a magnetic field, the viscosity of the MRF decreased distinctly; the sedimentation rate of MRF decreased from 58 to 3.5% after 100 days of sedimentation, and the migration distances of the MRFs were 22.4, 3.7, 2.4, and 0 mm, with particle sedimentation rates of 0.149, 0.019, 0.017, and 0 mm/h, respectively. The MRF with high dispersion stability was obtained, and the etching of CIP by HCl and the proper chain length of the coating of silane coupling agent were proved effective manners to improve the dispersion stability of MRF.

Effect of the difference water amounts and hydrolysis times of silane coupling agent on the shear bond strength between lithium disilicate glass ceramic and composite resin.

This study was to evaluate the effect of different water amounts and hydrolysis times of silane coupling agent on shear bond strength between lithium disilicate glass ceramic (LDS) and composite resin. Fourteen groups (n=7) of different water amounts (90, 50 and 10%v/v) and hydrolysis times (5, 19, 75 and 300 s) of experimental silane coupling agent that were prepared for silanization, non-silanization and commercial silane coupling agent (CSC) groups. Two-way analysis of variance (ANOVA) revealed no interaction between water amounts and hydrolysis times of ESC on shear bond strength between LDS and composite resin. One-way ANOVA exhibited the highest shear bond strength and the highest mean percentage in mixed failure mode in the 50%v/v group. Molecular analysis of 13C and 29Si indicated that nuclear magnetic resonance spectra of M2 and M3 hydrolysis species were found in 50%v/v group. The presenting of M2 and M3 which was predominant factor contributing to the highest shear bond strength.

Synthesis of Silane Functionalized LDH-Modified Nanopowders to Improve Compatibility and Enhance Corrosion Protection for Epoxy Coatings.

Novel modified Zn-Al LDH/epoxy coatings are synthesized and applied to steel substrates, providing active corrosion protection and improved barrier properties. This protective coating is made by combining Epon 828 as a polymer matrix with modified layered-double-hydroxy (LDH) nanoparticles acting as corrosion inhibitor containers. To synthesize the coatings, nitrate was intercalated into Zn-Al-LDH layers through an aqueous co-precipitation method to obtain Zn-Al LDH-NO3, and decavanadate replaced nitrate within the LDH layers through an anion exchange process to obtain Zn-Al LDH-(V10O28)6-. The intercalated LDH was functionalized by silanization with (3-aminopropyl)triethoxysilane (APTES) to increase the compatibility of the LDH inhibitor nanocontainers with epoxy resin and produce a protective coating. To protect the mild steel substrate, functionalized LDH nanopowders were dispersed into the epoxy resin, mixed with a polyamide hardener (Epikure 3571), and applied and cured to the metal surface. Surface morphology, structure, and chemical composition were determined for the modified LDH nanopowders using scanning electron microscopy, energy-dispersive X-ray analysis, X-ray diffraction, infrared spectroscopy, X-ray photoelectron spectroscopy, and thermogravimetric analysis. Corrosion protection of the coating system was studied using long-term immersion testing and potentiodynamic polarization studies in a 3.5 wt.% NaCl solution.

Influence of Silane Coupling Agent and Anionic Dispersant on the Dispersion Effect of Silicon Carbide Particles.

Silicon carbide (SiC), as a widely used material, has great properties. To improve the flowability of ultrafine silicon carbide slurry, this study used sodium humate, tetramethylammonium hydroxide (TMAH), and N-(ß-monoaminoethyl)-γ-aminopropyltrimethyl(ethoxysilane) (KH792) to modify the ultrafine silicon carbide powder produced by Qingzhou Micro Powder Company. The effects of different modifiers on improving the flowability of ultrafine silicon carbide slurry were investigated by means of viscosity tests, sedimentation experiments, and SEM observations. Their modification mechanisms were investigated by means of zeta potential tests, XPS tests, and so on. In this paper, the initial modification of SiC was carried out with KH792, followed by the secondary modification with anionic and cationic modifiers (tetramethylammonium hydroxide and sodium humate), and the optimal modification conditions were investigated by means of a viscosity test, which showed that the lowest viscosity of the modified SiC reached 0.076 Pa·s and that the absolute maximum value of the zeta potential increased from 47.5 at the time of no modification to 63.7 (maximum values) at the time of modification. This means it has an improved surface charge, which improves dispersion. The adsorption results of the modifier on the silicon carbide surface were also demonstrated by the XPS test results.

Shear bond strength of orthodontic brackets bonded to high-translucent dental zirconia with different surface treatments: An in vitro study.

PURPOSE: The objective of this study was to compare the shear bond strengths of orthodontic brackets bonded to translucent dental zirconia samples which are anatomically accurate and treated with various surface treatments. METHODS: This in vitro study included 156 samples from 3 brands of high-translucent zirconia split into a control group and 4 surface treatment groups: 9.6% hydrofluoric acid etching, 50-micron aluminium oxide particle air abrasion, and 30-micron tribochemical silica coating (TBS) particle air abrasion with and without silane application. After surface treatment, all groups were primed with a 10-MDP primer and bonded to metal orthodontic brackets. Shear bond strength (SBS) was tested and results were compared between all groups. Data analysis consisted of a balanced two-factor factorial ANOVA, a Shapiro-Wilks test, and a non-parametric permutation test. The significance level was set at 0.05. RESULTS: Among all surface treatments, aluminium oxide particle abrasion produced significantly higher SBS (P≤0.002). Lava™ Plus zirconia samples had significantly higher SBS than Cercon® samples (P<0.0001). TBS surface treatment produced significantly higher SBS on Lava™ Plus samples than it did on the other zirconia brands (P=0.032). CONCLUSIONS: This study indicated that mechanical abrasion using aluminium oxide in combination with a 10-MDP primer creates a higher SBS to high-translucent zirconia than the bond created by tribochemical silica coating. Also, there was no significant difference in ARI regardless of zirconia brand or surface preparation.

The Improvement of the Tribological Behaviour of Chemically Treated Abaca Fibre-Reinforced Polymer Composites.

Abaca fibres that have excellent mechanical properties are widely applied in the production and preparation of eco-friendly polymer composites as reinforcement materials. However, the weak interfacial bonding property of the abaca fibre and composite matrix limits the further extended application of abaca fibre-reinforced polymer composites. In this research, the findings demonstrate that, compared to raw abaca fibres, the interfacial shear strength (IFSS) value between the treated fibre and matrix is improved by 32% to 86%. Moreover, chemically treated abaca fibres could not only improve the wear resistance of the polymer composites, but also could promote the formation of primary and secondary plateaus. The best wear resistance behaviour was demonstrated by the sample with abaca fibres treated with 3% NaOH and 5% silane solutions, which had a maximum reduction in the sum wear rate of 28.44%. This research will provide detail on theoretical guidance and technical support for the development of eco-friendly natural fibre-reinforced polymer composites.

Effect of the Chemical Properties of Silane Coupling Agents on Interfacial Bonding Strength with Thermoplastics in the Resizing of Recycled Carbon Fibers.

Upcycling recycled carbon fibers recovered from waste carbon composites can reduce the price of carbon fibers while improving disposal-related environmental problems. This study assessed and characterized recycled carbon fibers subjected to sizing treatment using N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (APS) chemically coordinated with polyamide 6 (PA6) and polypropylene (PP) resins. Sizing treatment with 1 wt.% APS for 10 s yielded O=C-O on the surface of the carbon fiber, and the -SiOH in the APS underwent a dehydration-condensation reaction that converted O=C-O (lactone groups) into bonds of C-O (hydroxyl groups) and C=O (carbonyl groups). The effects of C-O and C=O on the interfacial bonding force increased to a maximum, resulting in an oxygen-to-carbon ratio (O/C) of 0.26. The polar/surface energy ratio showed the highest value of 32.29% at 10 s, and the interfacial bonding force showed the maximum value of 32 MPa at 10 s, which is about 15% better than that of commercial carbon fiber (PA6-based condition). In 10 s resizing treatments with 0.5 wt.% 3-methacryloxypropyltrimethoxysilane (MPS), C-O, C=O, and O=C-O underwent a dehydration-condensation reaction with -SiOH, which broke the bonds between carbon and oxygen and introduced a methacrylate group (H2C=C(CH3)CO2H), resulting in a significant increase in C-O and C=O, with an O/C of 0.51. The polar/surface free energy ratio was about 38% at 10 s, with the interfacial bonding force increasing to 27% compared to commercial carbon fiber (PP-based conditions). MPS exhibited a superior interfacial shear strength improvement, two times higher than that of APS, with excellent coordination with PP resin and commercial carbon fiber, although the interfacial bonding strength of the PP resin was significantly lower.

Surface-Modified Electrospun Glass Nanofibers from Silane Treatment and Their Use for High-Performance Epoxy-Based Nanocomposite Materials.

As a new and promising reinforcing filler, electrospun glass nanofibers (EGNFs) have attracted attention in the field of polymer composite materials. However, the reinforcing effectiveness of surface-modified EGNFs using different silane coupling agents in epoxy resin is still not quite clear. In this research, a series of silane coupling agents with increasing chain lengths in the order of methyl trimethoxysilane (MTMS), (3-aminopropyl) triethoxysilane (APTES), (3-glycidyloxypropyl) trimethoxysilane (GPTMS), and dual silane coupling agent APTES-GPTMS were employed to carry out surface treatment on the EGNFs. The pristine and silane functionalized EGNFs were then incorporated into epoxy resin as reinforcing fillers at low loading levels, i.e., 0.25 wt.%, 0.5 wt.%, and 1 wt.%, and the mechanical properties of the resultant epoxy nanocomposites, including strength, stiffness, ductility, and toughness, were evaluated. A commercial product of glass nanoparticles (GNPs) was used as a control to compare the reinforcing effectiveness of the EGNFs and the GNPs. This study revealed that the EGNFs could provide significant reinforcing and toughening effects at ultra-low loading (0.25 wt.%) in epoxy nanocomposite materials. Furthermore, surface modification of the EGNFs with silane coupling agents with long chain lengths, e.g., by using dual silane coupling agents, APTES-GPTMS, could enhance the interfacial bonding between the EGNFs and the epoxy matrix and further increase the mechanical performance of the EGNF-reinforced epoxy nanocomposite materials. Through this research, we realized epoxy nanocomposite materials with much-improved mechanical properties, i.e., 37%, 24%, 18%, 57% improvement in strength, stiffness, ductility, and toughness, respectively, with respect to those of the cured neat epoxy material with an ultra-low loading (0.25 wt.%) of APTES-GPTMS-EGNFs. Our research paves the road for developing lighter and stronger epoxy nanocomposite materials with EGNFs.

Mechanical Performance of Glass/Epoxy Composites Loaded with Silane-Treated Aluminum Hydroxide Fillers.

This study investigates the influence of silane-treated aluminum hydroxide on the mechanical performance of flame-retardant composites. These composites have potential applications for luggage bags, as a replacement for conventional plastics, offering more durability and lighter weight. Glass fabric was used as the reinforcement, while epoxy was used as the matrix material. To impart flame retardancy, aluminum hydroxide nanoparticles were used as fillers in different weight % age (5%, 10% and 15%). As these are inorganic particles and have compatibility issues with the matrix material, silane-coupling agents (Dynasylan® 6490 and Dynasylan Glymo) were used to treat these filler particles. Both the silane-coupling agents fraction used for treatment and the fillers fraction added to the composites were varied to determine the most optimum combination. The mechanical properties of the developed composites such as tensile, flexural, and short beam shear strength were investigated. The best results were exhibited by 10% aluminum hydroxide fillers treated with 1% (by weight) coupling agent (Dynasylan Glymo).

Effect of Different Silane Coupling Agents on Properties of Waste Corrugated Paper Fiber/Polylactic Acid Composites.

The surface of plant fibers was modified by silane coupling agents to prepare plant fiber/polylactic acid (PLA) composites, which can improve the dispersion, adhesion, and compatibility between the plant fibers and the PLA matrix. In this work, three silane coupling agents (KH550, KH560, and KH570) with different molecular structures were used to modify the surface of waste corrugated paper fibers (WFs), and dichloromethane was used as the solvent to prepare the WF/PLA composites. The effects of different silane coupling agents on the microstructure, mechanical properties, thermal decomposition, and crystallization properties of the composites were studied. The mechanical properties of the composites treated with 4 wt% KH560 were the best. Silane coupling agents can slightly improve the melting temperature of the composites, and WFs can promote the crystallization of PLA. The modification of WFs by silane coupling agents can increase the decomposition temperature of the WF/PLA composites. The content and type of silane coupling agent directly affected the mechanical properties of the WF/PLA composites. The interfacial compatibility between the WFs and PLA can be improved by using a silane coupling agent, which can further enhance the mechanical properties of WF/PLA composites. This provides a research basis for the further improvement of the performance of plant fiber/PLA composites.

Verification of Reinforced Surface Loose Layer of Zinc-Aluminum-Magnesium Steel Plate.

The corrosion resistance of zinc-aluminum-magnesium steel plates (Zn-Al-Mg steel plates) is significantly higher than that of galvanized steel plates. However, the unsatisfactory bonding performance of Zn-Al-Mg steel plates significantly limits their widespread application. In this study, X-ray photoelectron spectroscopy is employed to detect changes in the surface oxygen content of Zn-Al-Mg steel plates after different temperature treatments to confirm the existence of surface loose layers. In particular, changes in the surface oxygen content of the Zn-Al-Mg steel plates after the oxide layer is removed are investigated under saturated H2O vapor and O2 environmental conditions, and the cause of the formation of loose surface layers is determined. The uneven distribution of elements on the surface of the Zn-Al-Mg steel plates is investigated with scanning electron microscopy and energy dispersive spectroscopy. Nuclear magnetic resonance is employed to determine the size of the network spatial structure formed by silane coupling agents under different hydrolysis conditions and to further investigate the bonding performance of hydrolysate-modified Zn-Al-Mg steel plates. Several typical automotive adhesives are utilized to compare and examine the changes in the tensile strength of the Zn-Al-Mg steel plate bonding before and after modification with the silane coupling agent and analyze the structural damage of the adhesive at the bonding interface. The results confirm that the silane coupling agent strengthens the loose layer on the surface of the Zn-Al-Mg steel plate.

Poly-1,3-dioxolane anchoring graphitic carbon nitride to achieve high-energy-density solid-state Li metal batteries.

Solid-state Li metal batteries (SSLMBs) are promising solutions for the next-generation energy storage devices with high energy densities and safety. Accordingly, the advanced solid-state electrolytes are further needed to address the challenges-low ionic conductivity, poor interfacial compatibility and uncontrollably Li dendrites, boosting the electrochemical and safety performances of SSLMBs. Herein, a "flexible and rigid" strategy is proposed to enhance the electrochemical and mechanical properties of polyethylene oxide (PEO)-based electrolytes. Specifically, the flexible poly-1,3-dioxolane (poly-DOL) and rigid graphitic carbon nitride (g-C3N4) are coordinated by a coupling reaction to prepare g-C3N4-poly-DOL, which is further employed as the filler for the PEO matrix to fabricate a composite polymer electrolyte g-C3N4-pDOL-PEO. The flexible poly-DOL and rigid g-C3N4 together endow the PEO-based electrolyte with good interfacial stability, high ion-conductivity and strong mechanical strength. Consequently, the Li/g-C3N4-pDOL-PEO/LiFePO4 cell delivers high cyclability with a capacity retention ratio of 89.7 % after 150 cycles and an average Coulombic efficiency over 99.9 %, and, the Li/g-C3N4-pDOL-PEO/Li cell can stably cycle beyond 300 h at 0.2 mAh cm-2 with small polarization (13 mV). The "flexible and rigid" strategy coupling the polymer with the filler provides an effective electrolyte design for high-performance SSLMBs.

Efficient and sustainable photocatalytic inactivation of E. coli by an innovative immobilized Ag/TiO2 photocatalyst with peroxymonosulfate (PMS) under visible light.

A novel catalytic system for effective photocatalytic inactivation of Escherichia coli (E. coli) was constructed by anchoring Ag nanoparticles (AgNPs) on silane coupling agent (SCA) pretreated TiO2 nano-tube arrays (Ag/SCA/TiO2NTAs). Morphology and structural analyses revealed that SCA could disperse AgNPs evenly on TiO2NTAs, thus inducing a superior surface plasmon resonance (SPR) effect. Ag/SCA/TiO2NTAs catalyst exhibited excellent inactivation performance when in the presence of peroxymonosulfate (PMS) and visible light (VL), with 6-log E. coli was completely inactivated within 60 min, which was 5.3, 12.5 and 13.2 times higher than that of Ag/SCA/TiO2NTAs/VL, PMS/VL and Ag/SCA/TiO2NTAs/PMS/dark systems, respectively. Additionally, the photocatalyst exhibited a highly reusable property, with the inactivation performance almost unchanged after ten cycles of uses with minimal Ag leaching. The inactivation mechanism analysis demonstrated that both radical (SO4•-, OH) and non-radical (h+, 1O2) pathways involved in E. coli inactivation, and SCA played a pivotal role in the production of reactive species. Chloride ions (Cl-) greatly enhanced the inactivation efficiency, while bicarbonate (HCO3-) and phosphate (H2PO4-) showed an inhibitory effect. Humic acid (HA) displayed a dual effect on inactivation performance, where the low concentration of HA facilitated the bacteria inactivation, while the higher dose suppressed bacteria inactivation. Moreover, the system exhibited excellent inactivation performance in tap water. This work first used SCA as the binder to fix AgNPs on TiO2NTAs for VL photocatalytic inactivation of bacteria with the assistance of PMS, which was expected to provide some insights into the practical treatment of drinking water.

Bonding Characteristics of Silane Coupling Agent and MMA-Containing Primer to Various Composite CAD/CAM Blocks.

This study evaluated the bonding characteristics of a silane coupling agent (SCA) and a methyl methacrylate (MMA)-containing primer (MCP) for 11 types of commercial composite blocks (CBs) for sandblasted and non-sandblasted surfaces. The shear bond strength (SBS) was measured according to ISO 29022: Notched-edge shear bond strength test. The SBS results demonstrated statistically significant differences between the CBs under all identical conditions. For the non-sandblasted groups, the SBSs of MCP-treated specimens were significantly higher than those of SCA-treated specimens for all but two CBs. Comparing the two treatments in sandblasted groups, the SBS was significantly higher for seven out of 11 MCP-treated RCB specimens, in contrast with three cases for the SCA-treated group. Two-way ANOVA for SBS showed the interaction effect between sandblasting and primer type for specific CBs, indicating that the sandblasting treatment improved SBS more effectively for SCA-treated specimens. Moreover, the effect of the SCA treatment was more material-dependent compared to that of the MCP treatment, which did not achieve a strong bond in all CBs but proved more effective than the SCA treatment, especially for non-sandblasted surfaces.

Preparation of a Novel Formaldehyde-Free Impregnated Decorative Paper Containing MnO2 Nanoparticles for Highly Efficient Formaldehyde Removal.

The loading of catalytic manganese dioxide (MnO2) nanoparticles onto an impregnated decorative paper has been an effective method for the removal of indoor formaldehyde (HCHO) pollutants. However, its preparation can present numerous challenges, including instability in dipping emulsions and leaching. In this investigation, a novel and stable formaldehyde-free polyacrylate dipping emulsion containing MnO2 particles was prepared and then back-coated on a decorative paper. To improve the dispersion and fixation, the MnO2 was modified with silane. HCHO can undergo physical adsorption on the cellulosic fibers present in the paper, while it can also undergo chemical degradation into CO2 within the MnO2 groups. The silane not only enhanced the interfacial adhesion to a polyacrylate resin but also increased the interlayer distance, thereby creating a larger space for HCHO absorption. The impregnated decorative paper back-coated with 10 wt % of silane-modified MnO2 exhibited a removal efficiency of approximately 90% for HCHO at 20 °C. The removal rate further improved to approximately 100% when the temperature was increased to 60 °C. Moreover, it is worth noting that the release of volatile organic compounds was exceptionally minimal. Additionally, the particleboard bonded with this impregnated decorative paper exhibited an extremely low emission of HCHO, with a value that approached 0 mg·L-1. Furthermore, the bonding strength of the surface remained unaffected. Therefore, this study provides a simple and eco-friendly method for effectively removing HCHO, which can enhance indoor air quality.

Synergistic Improvement of Flame Retardancy and Mechanical Properties of Epoxy/Benzoxazine/Aluminum Trihydrate Adhesive Composites.

Epoxy resin was mixed with benzoxazine resin and an aluminum trihydrate (ATH) additive to provide flame retardancy and good mechanical properties. The ATH was modified using three different silane coupling agents and then incorporated into a 60/40 epoxy/benzoxazine mixture. The effect of blending compositions and surface modification on the flame-retardant and mechanical properties of the composites was investigated by performing UL94, tensile, and single-lap shear tests. Additional measurements were conducted including thermal stability, storage modulus, and coefficient of thermal expansion (CTE) assessments. The mixtures containing more than 40 wt% benzoxazine revealed a UL94 V-1 rating with high thermal stability and low CTE. Mechanical properties including storage modulus, and tensile and shear strength, also increased in proportion to the benzoxazine content. Upon the addition of ATH to the 60/40 epoxy/benzoxazine mixture, a V-0 rating was achieved at 20 wt% ATH. The pure epoxy passed a V-0 rating by the addition of 50 wt% ATH. The lower mechanical properties at high ATH loading could have been improved by introducing a silane coupling agent to the ATH surface. The composites containing surface-modified ATH with epoxy silane revealed about three times higher tensile strength and one and a half times higher shear strength compared to the untreated ATH. The enhanced compatibility between the surface-modified ATH and the resin was confirmed by observing the fracture surface of the composites.

Surface Modification of CaCO3 by Ultrasound-Assisted Titanate and Silane Coupling Agents.

Calcium carbonate (CaCO3) is a widely used inorganic powder, but its industrial applications are limited by its hydrophilicity and oleophobicity. Surface modification of CaCO3 can improve its dispersion and stability in organic materials and further improve its potential value. In this study, CaCO3 particles were modified with silane coupling agent (KH550) and titanate coupling agent (HY311) combined with ultrasonication. The oil absorption value (OAV), activation degree (AG), and sedimentation volume (SV) were employed to evaluate the modification performance. The results showed that the modification effect of HY311 on CaCO3 was better than that of KH550, and ultrasonic treatment played an auxiliary role. Based on response surface analysis, the optimal modification conditions were determined as follows: the HY311 dosage was 0.7%, the KH550 dosage was 0.7%, and ultrasonic time was 10 min. The OAV, AG, and SV of modified CaCO3 under these conditions were 16.65 g DOP/100 g, 99.27%, and 0.65 mL/g, respectively. The SEM, FTIR, XRD and thermal gravimetric analyses indicated successful coating of HY311 and KH550 coupling agents on the surface of CaCO3. The optimization of the dosages of two coupling agents and ultrasonic time improved the modification performance significantly.

Microscopic Origins of the Nonlinear Behavior of Particle-Filled Rubber Probed with Dynamic Strain XPCS.

The underlying microscopic response of filler networks in reinforced rubber to dynamic strain is not well understood due to the experimental difficulty of directly measuring filler network behavior in samples undergoing dynamic strain. This difficulty can be overcome with in situ X-ray photon correlation spectroscopy (XPCS) measurements. The contrast between the silica filler and the rubber matrix for X-ray scattering allows us to isolate the filler network behavior from the overall response of the rubber. This in situ XPCS technique probes the microscopic breakdown and reforming of the filler network structure, which are responsible for the nonlinear dependence of modulus on strain, known in the rubber science community as the Payne effect. These microscopic changes in the filler network structure have consequences for the macroscopic material performance, especially for the fuel efficiency of tire tread compounds. Here, we elucidate the behavior with in situ dynamic strain XPCS experiments on industrially relevant, vulcanized rubbers filled (13 vol %) with novel air-milled silica of ultrahigh-surface area (UHSA) (250 m2/g). The addition of a silane coupling agent to rubber containing this silica causes an unexpected and counterintuitive increase in the Payne effect and decrease in energy dissipation. For this rubber, we observe a nearly two-fold enhancement of the storage modulus and virtually equivalent loss tangent compared to a rubber containing a coupling agent and conventional silica. Interpretation of our in situ XPCS results simultaneously with interpretation of traditional dynamic mechanical analysis (DMA) strain sweep experiments reveals that the debonding or yielding of bridged bound rubber layers is key to understanding the behavior of rubber formulations containing the silane coupling agent and high-surface area silica. These results demonstrate that the combination of XPCS and DMA is a powerful method for unraveling the microscale filler response to strain which dictates the dynamic mechanical properties of reinforced soft matter composites. With this combination of techniques, we have elucidated the great promise of UHSA silica when used in concert with a silane coupling agent in filled rubber. Such composites simultaneously exhibit large moduli and low hysteresis under dynamic strain.