Effect of different CaSO4 contents on CaSiO3-CaSO4 porous composite bone scaffolds by 3D gel-printing

Porous CaSiO₃-CaSO₄ composite scaffolds were successfully prepared by 3D gel-printing (3DGP) technology in this study. In order to further improve the degradation performance of pure CaSiO₃ scaffolds, the effect of different CaSO₄ doping contents on CaSiO₃-CaSO₄ composite scaffolds was studied. The results show that when the porous composite scaffolds were placed in simulated body fluid (SBF) for 5 weeks, the weight loss rate was 2.41% (CaSiO₃-1%CaSO₄), 3.97% (CaSiO₃-3%CaSO₄), 4.18% (CaSiO₃-5%CaSO₄), 6.87% (CaSiO₃-7%CaSO₄), and 12.93% (CaSiO₃-9%CaSO₄), respectively, which could be concluded that CaSO₄ doping has a significant effect on improving the biodegradability of CaSiO₃ scaffolds. And CaSO₄ doping can also effectively improve the compressive strength of composite scaffolds and that of CaSiO₃-3%CaSO₄ composite scaffolds was tested as 54.67 MPa, and the shrinkage rate of porous composite scaffolds was nearly 11.4%, which meets the application requirements of bone repairing engineering.     

Effect of PCL concentration on PCL/CaSiO3 porous composite scaffolds for bone engineering

Porous polycaprolactone (PCL)-coated calcium silicate (CaSiO₃) composite scaffolds were successfully prepared by 3D gel-printing (3DGP) and vacuum impregnation technology in this study. The effect of different PCL concentration on porous CaSiO₃ scaffolds prepared by 3DGP technology was studied. The composition and morphological characteristics of PCL/CaSiO₃ scaffolds were tested by using fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM), and energy dispersive spectrometer (EDS) analysis. PCL coating amount on the scaffolds surface was calculated by thermogravimetric analysis (TGA). Compressive strength was tested by a universal testing machine, and degradability was tested by immersing the scaffolds in a simulated body fluid (SBF). The results show that PCL coating thickness increased from 7.29 μm to 12.2 μm, and the compressive strength of the corresponding composite scaffolds increased from 17.15 MPa to 24.12 MPa following with PCL concentration increasing from 7.5% to 12.5%. When the porous composite scaffolds were immersed in SBF for 28 days, the degradation ratio was 1.06% (CaSiO₃), 1.63% (CaSiO₃-7.5PCL), 1.81% (CaSiO₃-10PCL) and 1.55% (CaSiO₃-12.5PCL), respectively. It is obviously that PCL/CaSiO₃ composite scaffolds, which are suitable for bone growth in bone repair engineering, are beneficial to improve the mechanical properties and biodegradability of pure CaSiO₃ scaffolds.     

Preparation and characterisation of Fe/Fe3O4 fibres based soft magnetic composites

Soft magnetic composites (FSMCs) have been prepared by using Fe fibres coated with a layer of Fe₃O₄, this layer playing the role of insulating material. The coating was made via blackening method by simply immersing the fibres in the blackening bath for 5, 10 and 15 min. The formation of the Fe₃O₄ coating on the surface of the fibres was confirmed by X-ray diffraction. The SEM investigation, used to evaluate the thickness of the coatings, has proved that increasing the coating duration leads to the increase of the coating thickness and complete coverage of the surface of the fibres. Differential scanning calorimetry and thermomagnetic measurements were used to investigate the thermal stability of the composite fibres. The fibres coated with Fe₃O₄ were compacted at a compaction pressure of 700 MPa to obtain toroidal magnetic cores. The obtained cores were characterised in DC and AC magnetisation regime. The analysis of the quasi-static hysteresis loops evidenced that increasing the thickness of the Fe₃O₄ leads to a slight deterioration of the compact's magnetic properties. However, as the thickness of the Fe₃O₄ layer increases, the development of eddy currents at a larger scale is hindered as proved by the AC magnetic investigations. A model for analytic separation of the core losses is proposed. By applying this model to the prepared samples, we are now able to discriminate between the occurring losses and adjust the preparation process of new samples to the targeted characteristics.     

Crystallinity,conductivity, and magnetic properties of PVDF‐Fe3O4 composite films

The formation of Fe₃O₄ nanoparticles by hydrothermal process has been studied. X‐ray Diffraction measurements were carried out to distinguish between the phases formed during the synthesis. Using the synthesized Fe₃O₄ nanoparticles, poly(vinyledene fluoride)‐Fe₃O₄ composite films were prepared by spin coating method. Scanning electron microscopy of the composite films showed the presence of Fe₃O₄ nanoparticles in the form of aggregates on the surface and inside of the porous polymer matrix. Differential Scanning calorimetry revealed that the crystallinity of PVDF decreased with the addition of Fe₃O₄. The conductitivity of the composite films was strongly influenced by the Fe₃O₄ content; conductivity increased with increase in Fe₃O₄ content. Vibration sample magnetometry results revealed the ferromagnetic behavior of the synthesized iron oxide nanoparticles with a Ms value of 74.50 emu/g. Also the presence of Fe₃O₄ nanoparticles rendered the composite films magnetic. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

In situ preparation of magnetic Fe3O4.Cu2O.Fe3O4/cryogel nanocomposite powder via a reduction–coprecipitation method as adsorbent for methylene blue water pollutant

Magnetic nanocomposites have attracted great attention as adsorbents for the removal of water pollutants, which respond to an external magnet that is used to remove both pollutants and composite nanomaterial traces from water. They are environmentally friendly and effective adsorbents for water treatment. In this respect, a simple in situ preparation method was used to prepare cryogel powder composite based on Fe₃O₄.Cu₂O.Fe₃O₄ nanomaterials. The ionic cryogel based on 2‐acrylamido‐2‐methylpropane sulfonate sodium salt and styrene sulfonate sodium salt was prepared by crosslinking polymerization at low temperature. The new magnetic nanoparticles based on Fe₃O₄.Cu₂O.Fe₃O₄ were successfully prepared inside the cryogel networks by a simple reduction–coprecipitation method based on reaction of Fe³⁺ with sodium sulfite and Cu²⁺ in the presence of hydroxylamine and ammonia solution. The thermal stability, accurate Fe₃O₄.Cu₂O.Fe₃O₄ content, magnetic properties, crystal lattice structure, particle sizes and morphology of the prepared cryogel composite were evaluated. The optimum conditions such as pH, contact time, adsorbate concentrations, adsorption equilibrium and adsorption kinetics were investigated to determine the efficiency of the prepared composite as an adsorbent to remove toxic methylene blue (MB) pollutant from aqueous solution. The data for MB adsorption confirmed the high ability of the prepared composite to remove more than 4.696 mmol L^?1 of MB from water during 6 min. The regeneration and reuse experiments showed excellent data for the synthesized new dye as an effective adsorbent for water treatment. © 2018 Society of Chemical Industry     

Effect of different dopants on porous calcium silicate composite bone scaffolds by 3D gel-printing

Porous CaSiO₃ composite scaffolds with different dopants, such as MgSiO₃, MgCl₂ and CaSO₄, were successfully prepared by 3D gel-printing (3DGP). (m, n) is proposed to describe the filament geometry features. The results show that doping can improve the strength of porous composite scaffolds and MgCl₂-doped composite scaffolds had the highest modulus of elasticity of 1241 MPa. The shrinkage rate range of the composite scaffolds was 11.44–13.16%, and their porosity was all about 60%. When porous composite scaffolds were soaked in SBF for 28 days at 37°С, the degradation rate was 2.7% (pure), 0.3% (MgSiO₃), 0.2% (MgCl₂), 5.27% (CaSO₄), respectively. It explains that MgSiO₃ and MgCl₂ inhibited the in vitro degradation of CaSiO₃, while CaSO₄ promoted. It is obviously that doped MgCl₂ can improve the mechanical properties of porous scaffolds, and doped CaSO₄ can improve the degradation of scaffolds, which play an important role in bone repair engineering.     

Fabrication of PLA/MWCNT/Fe3O4 composite nanofibers for leukemia cancer cells

The efficient delivery of daunorubicin loaded poly (lactic acid) (PLA)/multiwalled carbon nanotubes (MWCNT)/Fe₃O₄ composite nanofibers was investigated. The synthesized nanofibers were characterized using SEM, TEM, and XRD analysis. The proliferation inhibition effect of PLA/MWCNT/Fe₃O₄ nanofibrous scaffolds on leukemia K562 cell lines was investigated. The effect of nanofiber concentration on the daunorubicin delivery in the absence and presence of external magnetic field was also evaluated. The results indicated that the incorporation of daunorubicin into the prepared nanofibrous scaffold under applied magnetic field could have synergistic cytotoxic effect on leukemia cancer cells. The drug release mechanism followed the non-Fickian transport.     

Controlled preparation of Fe3O4/P (St-MA) magnetic composite microspheres by DPE method

In this work, controlled radical polymerization based on 1, 1-diphenylethylene (DPE method) was used to prepare magnetic composite microspheres. By this method, Fe₃O₄/P (St-MA) magnetic composite microspheres were prepared via copolymerization of styrene (St) and maleic anhydride (MA) using DPE as radical control agent in the presence of Fe₃O₄ nanoparticles. The structure and properties of the magnetic composite microspheres obtained were characterized by IR, ¹H-NMR, SEC-MALLS, TEM, TGA, VSM, DLS and other instruments. It was found that the DPE method allows the controlled preparation of magnetic composite microspheres, and Fe₃O₄/ P(St-MA) microspheres possess perfect sphere-shaped morphology, homogeneous particle size, carboxylic surface, superparamagnetism with a saturation magnetization of 14.704 emu/g, and magnetic content with a value of 25%.     

Effect of different MgFe2O4 contents on 3D gel-printed porous TCP–MgFe2O4 composite scaffolds

Magnetic materials have shown significant influence in the process of bone regeneration. In order to combine the bone repairing capability of tricalcium phosphate (TCP) ceramic with magnetic material, porous TCP–MgFe₂O₄ composite scaffolds were successfully prepared by three-dimensional (3D) gel-printing technology, and the effect of different MgFe₂O₄ contents on TCP–MgFe₂O₄ composite scaffolds was studied. The viscosity of printing slurry prepared with polyvinyl alcohol as binder decreased with the increase of shear rate, showing shear thinning. Results show that following with MgFe₂O₄ content increasing from 30 to 70 wt%, the compressive strength of the composite scaffolds increased from 8.45 to 10.58 MPa, the saturation magnetization increased from 3.07 to 7.20 emu/g, and the weight loss rate of degradation in vitro increased from 1.83% to 2.1% after 4 weeks, respectively. Live and dead staining shows that MC3T3-E1 cells had better proliferation on TCP–MgFe₂O₄ composite scaffolds than TCP scaffolds. Compared with pure TCP scaffolds, the addition of MgFe₂O₄ improves the comprehensive performance of scaffolds and meets the application requirements of bone repairing.     

Magnetic and conducting Fe3O4–polypyrrole nanoparticles with core‐shell structure

Magnetic and conducting Fe₃O₄–polypyrrole nanoparticles with core‐shell structure were prepared in the presence of Fe₃O₄ magnetic fluid in aqueous solution containing sodium dodecylbenzenesulfonate (NaDS) as a surfactant and dopant. Both the conductivity and magnetization of the composites depend strongly on the Fe₃O₄ content and the doping degree. With increase of Fe₃O₄ content in the composite, the conductivity at room temperature decreases, but the saturated magnetization and coercive force increase. Transmission electron microscopy (TEM) images of Fe₃O₄ and Fe₃O₄–polypyrrole particles show almost spherical particles with diameters ranging from 20 to 30 and 30 to 40 nm, respectively. The thermal stability of Fe₃O₄–polypyrrole composites is higher than that of pure polypyrrole. Studies of IR, UV–visible and X‐ray photoelectron spectroscopy (XPS) spectra suggest that the increased thermal stability may be due to interactions between Fe₃O₄ particles and polypyrrole backbone. Copyright © 2003 Society of Chemical Industry     

Magnetic-field-induced Fe3O4@CNTs/PES/SPSf composite membrane for efficient removal of methylene blue by adsorption and catalytic degradation

Novel composite membranes are successfully developed for adsorption and catalytic degradation of methylene blue (MB) by blending Fe₃O₄-coated CNTs (Fe₃O₄@CNTs) nanoparticles in polyethersulfone (PES) and sulfonated polysulfone (SPSf) matrix via nonsolvent-induced phase separation (NIPS) method assisted by magnetic field. Fe₃O₄@CNTs nanoparticles migrate to the separation layer under the induction of magnetic field, thus Fe₃O₄@CNTs/PES/SPSf composite membranes prepared under magnetic field exhibit a better dye removal ability compared with that without magnetic field. The MB removal ratio by Fe₃O₄@CNTs/PES/SPSf composite membrane containing 8 wt% Fe₃O₄@CNTs (M2−M) can reach up to 99% in 30 min under the conditions of 0.25 g composite membrane, 20 mg/L MB, 0.1 mol/L H₂O₂, pH = 3 and 80°C. Furthermore, the composite membranes show excellent recycling performance, as the MB removal capacity remains at 99% even after four cycles.     

Synthesis and characterization of novel conducting composites of Fe3O4 nanoparticles and sulfonated polyanilines

Surface charged iron oxide (Fe₃O₄) nanoparticles were used for the synthesis of sulfonated polyaniline (SPAN)‐Fe₃O₄ nanocomposites (SPAN/Fe₃O₄‐NCs). 2,5‐diaminobenzenesulfonic acid (DABSA) and 2‐aminobenzenesulfonic acid (ABSA) were independently polymerized with aniline to form SPAN. The structure of the composites was characterized by means of transmission electron microscopy (TEM), X‐ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectra, conductivity and magnetic properties. TEM reveals that Fe₃O₄ nanoparticles are “glued” with SPAN in the composite. TGA indicates that SPAN/Fe₃O₄‐NCs are having better thermal stability. The room temperature conductivity of SPAN/Fe₃O₄‐NCs is higher than that of pristine PANI and SPAN. SPAN/Fe₃O₄‐NCs exhibits magnetic behavior. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 4127–4134, 2007     

Template synthesis and magnetic response of polyaniline/Fe3O4 composite microtubes

Template synthesis technique was employed to prepare magnetic polyaniline (PANI)/Fe₃O₄ composite microtubes using anodic aluminum oxide (AAO) membrane as template. Magnetic microtubes were obtained through in situ polymerization of aniline in the presence of Fe₃O₄ nanoparticles in the microchannels of template. A tubular structure was formed once when aniline was preferentially adsorbed and polymerized on the surface of channels wall. Electron microscope images demonstrated that the shape and size of guest (PANI/Fe₃O₄ composite microtubes) were strictly depended on those of the host (template channels). Magnetic force microscopy images showed that the PANI/Fe₃O₄ composite microtubes possessed reasonable magnetism and the magnetism distribution of microtubes was regular as distribution of template channels. Moreover, the magnetic response and oriented arrangement of PANI/Fe₃O₄ microtubes were fulfilled in the magnetic field. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Preparation of novel hydrophobic magnetic Fe3O4/waterborne polyurethane nanocomposites

Magnetic Fe₃O₄/waterborne polyurethane nanocomposites were synthesized based on waterborne polyurethane (WPU) and amino-functionalized Fe₃O₄ by in situ polymerization. The Fe₃O₄ nanoparticle was found to be uniformly distributed in Fe₃O₄/WPU nanocomposites with linear or crosslinked structure. In addition, the formation mechanism and magnetic conduction mechanism of stable inorganic–organic nanocomposites were discussed. The experimental results showed that the thermal stability, magnetic, and mechanical properties of magnetic Fe₃O₄/waterborne polyurethane nanocomposites were improved by amino functionalized Fe₃O₄. Furthermore, the defoaming property of the emulsion and the hydrophobic property of magnetic Fe₃O₄/waterborne polyurethane nanocomposites were improved by the 1-hexadecanol-terminated prepolymer. What more, polycaprolactone (PCL)-based Fe₃O₄/WPU nanocomposites have excellent mechanical properties (The tensile strength is over 30 MPa, the elongation rate is above 300%.) and magnetic properties. Magnetic Fe₃O₄/waterborne polyurethane nanocomposites will be used in the field of hydrophobic and microwave absorbent materials. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 48546.     

Effects of organic encapsulation on the properties of magnetic PLLA/Fe3O4 composites

Organic‐encapsulated Fe₃O₄ magnetic microspheres (MMS) were synthesized and used to prepare PLLA (poly (L ‐lactic acid))/MMS composites. The effects of organic encapsulation on the mechanical, thermal, and magnetic properties of the composites were investigated. When compared with the PLLA/Fe₃O₄ composite, the elongation ratio of the PLLA/MMS composite improved significantly (by nearly 300%). Scanning electron microscope (SEM) images of the fracture morphology revealed an interesting “silking” phenomenon within the PLLA/MMS composite, which explains the greatly improved toughness. The decreased crystallinity and increased thermal stability of the PLLA/MMS composite suggest the existence of strong interacting forces between the PLLA molecules and the organic layer of the MMS particles, thereby limiting the mobility of the macromolecular chains. A study of the composites' magnetic properties indicated that the saturation magnetization was determined by the relative Fe₃O₄ content in the matrix, but not the types of the filling particles. POLYM. ENG. SCI., 2009. © 2009 Society of Plastics Engineers     

Carboxyl‐containing polyarylene ether nitrile/Fe3O4 hybrids and their effects on the PEN composites

In this study, the novel polyarylene ether nitrile containing carboxyl groups (CPEN)/Fe₃O₄ hybrids were synthesized via the solvent‐thermal route. The SEM and TEM images showed that the surface of functionalized Fe₃O₄ hybrids (CPEN‐f‐Fe₃O₄) became rough and coated with a thin polymer layer successfully. Chemical bonds were formed between the carboxyl groups and Fe₃O₄ spheres, which were characterized by FTIR and XRD. Series of PEN composite films were prepared through solution‐casting method with different contents of CPEN‐f‐Fe₃O₄ hybrids and raw Fe₃O₄ spheres. The SEM images showed that the CPEN‐f‐Fe₃O₄ hybrids became much more dispersible and compatible in PEN matrix than that of raw Fe₃O₄ spheres, which was further confirmed by rheological study. The magnetic analysis showed that the saturation magnetization of composites films increased with the increase of CPEN‐f‐Fe₃O₄ hybrids loading content. The results of thermogravimetric and mechanical study exhibited that the composite films had good thermal stability and mechanical property. POLYM. COMPOS., 36:1325–1334, 2015. © 2014 Society of Plastics Engineers     

Nucleation mechanism and morphology of polystyrene/Fe3O4 latex particles via miniemulsion polymerization using AIBN as initiator

In this study, oil‐based magnetic Fe₃O₄ nanoparticles were first synthesized by a coprecipitation method followed by a surface modification using lauric acid. Polystyrene/Fe₃O₄ composite particles were then prepared via miniemulsion polymerization method using styrene as monomer, 2,2′‐azobisisobutyronitrile (AIBN) as initiator, sodium dodecyl sulfate (SDS) as surfactant, hexadecane (HD) or sorbitan monolaurate (Span20®) as costabilizer in the presence of Fe₃O₄ nanoparticles. The effects of Fe₃O₄ content, costabilizer, homogenization energy during ultrasonication, and surfactant concentration on the polymerization kinetics (e.g., conversion), nucleation mechanism, and morphology (e.g., size distributions of droplets and latex) of composite particles were investigated. The results showed that at high homogenization energy, an optimum amount of SDS and hydrophobic costabilizer was needed to obtain composite particles nucleated predominately by droplet nucleation mechanism. The morphology of the composite particles can be well controlled by the homogenization energy and the hydrophobicity of the costabilizer. The magnetic composite particles can be made by locating Fe₃O₄ inside the latex particles or forming a shell layer on their PS core surface depending on the aforementioned polymerization conditions. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and characterization of (Fe3O4/MWCNTs)/ epoxy nanocomposites

A sonochemical technique is used for in situ coating of iron oxide (Fe₃O₄) nanoparticles on outer surface of MWCNTs. These Fe₃O₄/MWCNTs were characterized using a high‐resolution transmission electron microscope (HRTEM), X‐ray diffraction, and thermogravimetric analysis. The as‐prepared Fe₃O₄/MWCNTs composite nanoparticles were further used as reinforcing fillers in epoxy‐based resin (Epon‐828). The nanocomposites of epoxy were prepared by infusion of (0.5 and 1.0 wt %) pristine MWCNTs and Fe₃O₄/MWCNTs composite nanoparticles. For comparison purposes, the neat epoxy resin was also prepared in the same procedure as the nanocomposites, only without nanoparticles. The thermal, mechanical, and morphological tests were carried out for neat and nanocomposites. The compression test results show that the highest improvements in compressive modulus (38%) and strength (8%) were observed for 0.5 wt % loading of Fe₃O₄/MWCNTs. HRTEM results show the uniform dispersion of Fe₃O₄/MWCNTs nanoparticles in epoxy when compared with the dispersion of MWCNTs. These Fe₃O₄/MWCNTs nanoparticles‐infused epoxy nanocomposite shows an increase in glass transition (T_g) temperature. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Fe3O4@mesoporouspolyaniline: A Highly Efficient and Magnetically Separable Catalyst for Cross‐Coupling of Aryl Chlorides and Phenols

A high surface, magnetic Fe₃O₄@mesoporouspolyaniline core‐shell nanocomposite was synthesized from magnetic iron oxide (Fe₃O₄) nanoparticles and mesoporouspolyaniline (mPANI). The novel porous magnetic Fe₃O₄ was obtained by solvothermal method under sealed pressure reactor at high temperature to achieve high surface area. The mesoporouspolyaniline shell was synthesized by in situ surface polymerization onto porous magnetic Fe₃O₄ in the presence of polyvinylpyrrolidone (PVP) and sodium dodecylbenzenesulfonate (SDBS), as a linker and structure‐directing agent, through ‘blackberry nanostructures’ assembly. The material composition, stoichiometric ratio and reaction conditions play vital roles in the synthesis of these nanostructures as confirmed by variety of characterization techniques. The role of the mesoporouspolyaniline shell is to stabilize the porous magnetic Fe₃O₄ nanoparticles, and provide direct access to the core Fe₃O₄ nanoparticles. The catalytic activity of magnetic Fe₃O₄@mesoporousPANI nanocomposite was evaluated in the cross‐coupling of aryl chlorides and phenols.     

Influence of Fe3O4 nanoparticles decoration on dye adsorption and magnetic separation properties of Fe3O4/rGO nanocomposites

Magnetite (Fe₃O₄) nanoparticles were prepared by solvothermal method and its composites with reduced graphene oxide namely FG1, FG2, and FG3 (changing magnetite precursor loading 0.1, 0.5, and 1 respectively) were used as adsorbents for the removal of methyl violet (MV) dye. The structural and morphological results confirm that rGO sheets were decorated with Fe₃O₄ and it ensures the variation of active sites toward dye removal property. The maximum adsorption capacity obtained for FG2 was 196 mg/g. The adsorption isotherms and kinetics better fit Langmuir and pseudo-second-order kinetic model for FG1 and FG2. Increasing of Fe₃O₄ loading on rGO reduces the dye adsorption sites and too low Fe₃O₄ loading affects the magnetic separation. The optimal loading of Fe₃O₄ on rGO is important parameter for the adsorption process and fast separation of adsorbent.