Effects of formaldehyde solution and nanoparticles on mechanical properties and biodegradation of gelatin/nano β-TCP scaffolds

In this study, gelatin/beta tricalcium phosphate (β-TCP) nanocomposite scaffolds were prepared by solvent casting method. The cross-linking method was carried out by adding formaldehyde to gelatin. The microparticles of sodium chloride were used as porogen agent. Characterization of nano β-TCP was performed using XRD, FTIR, and SEM. Results showed that the size of the particles is about 100 nm with spherical morphology. In addition, the scaffold characterization was carried out using FTIR and SEM techniques. Observations showed a porous texture with pore size between 100 and 400 μm. The biodegradability and bioactivity evaluations of the scaffolds were done by immersing them in a simulated body fluid solution for different time periods. The biodegradability studies demonstrated a reduction in the degradation rate of gelatin/β-TCP nanocomposite scaffolds due to the presence of β-TCP nanoparticles. The obtained results of bioactivity tests confirmed the formation of apatite layer on the surface of the scaffolds. Furthermore, the effects of porosity, cross-linking agent, and β-TCP nanoparticles on the bending and compressive properties of the composite scaffolds were examined. According to the mechanical examinations of the scaffolds, the best bending and compressive properties occurred in the presence of 10 and 20 wt% of β-TCP nanoparticles, respectively. The appropriate mechanical properties and biodegradation rate for tissue engineering applications obtained at 1 g of the formaldehyde solution.     

Enhancement of mechanical strength and osteogenesis,and inhibition of osteoclastic activity for β-tricalcium phosphate bioceramics by incorporating calcium silicate and magnesium-strontium phosphate

β-tricalcium phosphate bioceramics suffer from a drawback of poor mechanical strength and a scarcity of capacity to regulate biological performances. In the current study, the overall performances of β-tricalcium phosphate (TCP) bioceramics were improved by incorporating calcium silicate (CS) and magnesium-strontium phosphate (MSP). During the sintering process, the MSP stabilized the β phase of TCP, and the formation of MSP melt ensured effective liquid-sintering of TCP, thus conducing to lower porosity of TCP/MSP and TCP/CS/MSP bioceramics. In comparison with the TCP bioceramics, the TCP/CS and TCP/MSP bioceramics showed lower compressive strength, while the TCP/CS/MSP bioceramics attained noticeably higher compressive strength. Due to the sustained release of therapeutical ions, the TCP/CS bioceramics enhanced in vitro early-stage osteoblastic differentiation, but compromised cell proliferation; both the TCP/MSP and TCP/CS/MSP bioceramics enhanced cell proliferation and osteoblastic differentiation, and restrained osteoclastic activities. Collectively, the TCP/CS/MSP bioceramics with optimal overall performances are promising for efficaciously treating the defects of osteoporotic bone.     

Effects of Mn-doping on the structure and in vitro degradation of β-tricalcium phosphate

β-tricalcium phosphate (β-TCP) is an ideal biomaterial for the bone repair because of its biocompatibility and biodegradability. In this study, 0 mol%, 5 mol%, 15 mol% and 30%mol bivalent manganese ion (Mn²⁺) doped β-TCP (Mn-TCP) powders were synthesized by a sol-gel method. The amount of the dopants significantly influences the crystallinity and the parameters related with structure of β-TCP, such as the lattice parameters and crystallite dimensions. The particle size and the particle distribution of doped β-TCP powers were evaluated as well. Meanwhile, the as-synthesized powders were consolidated by sintering at 1000 °C in muffle furnace for 5 h to get Mn-TCP porous material and the degradation experiment was carried out in Simulated Body Fluid (SBF) solution for 28 days. Then, Mn-TCP porous material were characterized by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscope (SEM). Significantly, there were bone-like apatite materials deposited on the surface of bone-like porous materials. With the increasing doping amount of Mn²⁺, the newly formed apatite-like materials decreased, while the crystallinity increased significantly. Besides, pH results showed that alkaline environment was more favorable for the formation of sedimentary materials.     

Synthesis and characterization of β-TCP/CNT nanocomposite: Morphology,microstructure and in vitro bioactivity

In this study, β-TCP/CNT nanocomposite has been synthesized by solution precipitation method. Then, the effects of the different percentage of CNT (CNT1β-TCP, CNT3β-TCP, CNT5β-TCP) and surfactant (CNT1β-TCP1SDBS, CNT1β-TCP2SDBS, CNT1β-TCP3SDBS) on β-TCP/CNT nanocomposite powder were studied. The X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) analyses were used to characterize the samples. The observations revealed that the microstructure of 1 wt% CNT could provide dispersion without agglomeration in nanocomposite powder; however, a higher concentration of CNT powder in the nanocomposite resulted in the formation of Ca₂PO₇ phase. Implementing 2 wt% of SDBS as a surfactant modified the shape, size, and distribution of CNT particles on nanocomposites. Finally, the nanocomposite sample was immersed in simulated body fluid (SBF) to evaluate the in vitro bioactivity. It obviously showed an apatite layer on the surface after 7 days of immersion in SBF. Taken together, this nanocomposite might be potentially to be used as bone repair biomaterial.     

Biphasic calcium phosphate (BCP) macroporous scaffold with different ratios of HA/β-TCP by combination of gel casting and polymer sponge methods

Abstract

Open and interconnected porous scaffolds were prepared with various ratios of hydroxyapatite (HA)/β-tricalcium phosphate by a combination of gel casting and polymer sponge methods to improve the mechanical properties and structure. The scaffolds were prepared using slurries containing 50 vol.-% of ceramic powders and sintered at 1100°C for 2 h. Thermogravimetric analysis result shows that the proper temperature to burn out organic materials and polyurethane foams is 600°C. The compressive strength was between 5·3 and 8·4 MPa. Field emission scanning electron microscope shows an open, relatively uniform and large interconnected porous structure with pore size ranging between 150 and 400 μm. X-ray diffraction and Brunauer–Emmett–Teller methods were employed to determine the microstructural crystallite and surface area respectively. The results show that the compressive strength of scaffolds increased with the increase in HA concentration. The reason can be explained by the increasing pore wall thickness and density in scaffolds.     

Structural,magnetic and dielectric properties of Co-Zr substituted M-type calcium hexagonal ferrite nanoparticles in the presence of α-Fe2O3 phase

Polycrystalline nanoparticles of M-type Ca(ZrCo)_xFe_12?2xO₁₉ (0.0?≤?x?≤?1.0) hexaferrites were prepared using a simple heat treatment method at a low heating temperature of 650?°C. Effect of cobalt-zirconium substitution on the structural, microstructural, magnetic and dielectric properties was investigated. XRD analysis indicates that all the samples possess a hexagonal structure with anti-ferromagnetic α-Fe₂O₃ phase. The values of lattice parameters and cell volume found to be increased with increasing the cobalt-zirconium substitution along with the amount of α-Fe₂O₃ phase. Crystal symmetry has not affected by Zr–Co substitution in prepared calcium hexaferrite samples but the position of diffraction peak [108] is found to shift towards a lower angle as an increase in the substitution of Zr–Co. The crystallite size found to vary between 12 and 17?nm. SEM images show agglomerated grains and surface morphology has changed with Zr–Co substitution. EDX analysis of typical samples revealed the presence of Ca, Fe, Co, Zr. The magnetic analysis revealed the formation of multi-domain structure. Room temperature Mössbauer spectra of prepared samples show that all five sextets are merged together with a paramagnetic doublet and it confirmed that the size of particles is very small in the nano range. Single and double semicircle arcs were observed in Cole-Cole plots, due to the contributions of grain and grain boundaries resistance.     

Evaluation of hydroxyapatite and β-tri calcium phosphate microplasma spray coated pin intra-medullary for bone repair in a rabbit model

Here we report a comparative study of the healing kinetics of surgically created artificial defects in the tibia of New Zealand white rabbits. Comparison of the healing kinetics was made for uncoated conventional SS316L intramedullary pins, and the same pins with microplasma sprayed (MIPS) pure hydroxyapatite (HAp) and beta-tri calcium phosphate (β-TCP) coatings. After thorough material characterizations including XRD, FTIR, SEM, etc., MIPS coated pins were implanted to such animals. Serum biochemistry, radiology and fluorochrome labelling were used to evaluate the comparative healing kinetics of these implants in vivo. In comparison to those of the uncoated pins, the pins coated with both MIPS HAp and β-TCP showed significant increment of alkaline phosphatase up to 15th postoperative day, insignificant changes in serum phosphorus and calcium with uneventful healing of bone defect. There was development of Havarsian canals and well-defined peripherally placed osteoblasts along with evidence of angiogenesis and comparatively more new bone formation in the defect site. On a comparative scale, the performance of the β-TCP coated intramedullary pins was much better than that of the pure HAp coated pins than the uncoated intramedullary pins.     

Enhanced magnetic,ferroelectric, and photocatalytic properties of (1-x)BiFeO3-xBaTiO3 (0.0 ≤ x ≤ 0.4) powders

The magnetic, ferroelectric, and photocatalytic properties of (1-x)BiFeO₃-xBaTiO₃ (0.0 ≤ x ≤ 0.4) powders synthesized by sol-gel method have been investigated. X-ray diffractometry confirms that the phase of the samples changed from rhombohedral to cubic with the increase in BaTiO₃ content. The grain size decreases and the particle shape becomes homogeneous with the introduction of BaTiO₃. BaTiO₃ substitution enhances the multiferroic properties of the ceramics and the maximum remnant magnetization (0.261 emu/g) and remnant polarization (20 μC/cm²) have acquired in 0.8BiFeO₃-0.2BaTiO₃ and 0.7BiFeO₃-0.3BaTiO₃, respectively. The absorbance in ultraviolet and visible light regions is improved obviously for powder with x = 0.3. The energy band gap of the samples decreases from 2.06 eV to 1.57 eV with the introduction of BaTiO₃, indicating that the excitation rate of photogenerated electron-hole pairs is improved. The highest methylene blue degradation efficiency of ~62% within 3 h under the visible light is achieved in the 0.7BiFeO₃-0.3BaTiO₃ which can be attributed to its suitable energy band gap and large remnant polarization.     

Static magnetic field-assisted synthesis of Fe_3O_4 nanoparticles and their adsorption of Mn(Ⅱ) in aqueous solution

A facile method for synthesis of the magnetic Fe_3O_4 nanoparticles was introduced.Magnetic nanoparticles were prepared via co-precipitation method with(PMF) and without(AMF) 0.15 T static magnetic field.The effects of magnetic field on the properties of magnetic nanoparticles were studied by XRD,TEM,SEM,VSM and BET.The results showed that the magnetic field in the co-precipitation reaction process did not result in the phase change of the Fe_3O_4 nanoparticles but improved the crystallinity.The morphology of Fe_3O_4 nanoparticles was varied from random spherical particles to rod-like cluster structure.The VSM results indicated that the saturation magnetization value of the Fe_3O_4 nanoparticles was significantly improved by the magnetic field.The BET of Fe_3O_4nanoparticles prepared with the magnetic field was larger than the control by 23.5%.The batch adsorption experiments of Mn(Ⅱ) on the PMF and AMF Fe_3O_4 nanoparticles showed that the Mn(II) equilibrium capacity was increased with the pH value increased.At pH 8,the Mn(Ⅱ) adsorption capacity for the PMF and AMF Fe_3O_4 was reached at 36.81 and 28.36 mg·g~(-1),respectively.The pseudo-second-order model fitted better the kinetic models and the Freundlich model fitted isotherm model well for both PMF and AMF Fe_3O_4.The results suggested that magnetic nanoparticles prepared by the magnetic field presented a fairly good potential as an adsorbent for an efficient removal of Mn(Ⅱ) from aqueous solution.     

New dinuclear cobalt (ΙΙ, ΙΙΙ) and tetranuclear manganese (ΙΙΙ) complexes assembled by a polydentate Schiff-base ligand: synthesis,structure and magnetic properties

The reactions of 2-(((2-hydroxy-3-methoxyphenyl)methylene)amino)-2-(hydroxymethyl)-1,3-propanediol (H₄L) and Mn(ClO₄)₂·6H₂O or Co(SCN)₂·3H₂O in the presence of triethylamine in methanol led to the formation of two new complexes [Mn^ΙΙΙ₄(HL)₂(H₂L)₂(CH₃OH)₄]·4CH₃OH·(ClO₄)₂ (1) and [Co^ΙΙCo^ΙΙΙ(H₂L)₂(CH₃OH)(SCN)]·1.5CH₃OH·1.5H₂O (2), respectively. According to structural data and magnetic properties tetranuclear complex 1 contains four homo-valence manganese (ΙΙΙ) atoms, while in the binuclear complex 2 composed of hetero-valence bi- and trivalent cobalt (ΙΙ, ΙΙΙ) atoms. Weak antiferromagnetic exchange interactions between neighboring manganese ions in 1 have place. χ_MT for 2 was fitted using a model of isolated cobalt (ΙΙ) ion with zero-field splitting parameters and the study confirms its mixed valence Co^ΙΙ/Co^ΙΙΙ nature. No slow magnetic relaxation effects were observed for both complexes in the absence of an applied dc magnetic field.     

Production, mechanical properties and in vitro biocompatibility of highly aligned porous poly(ε-caprolactone) (PCL)/hydroxyapatite (HA) scaffolds

We produced highly aligned porous poly(ε-caprolactone) (PCL)/hydroxyapatite (HA) scaffolds by unidirectionally freezing PCL/HA solutions with various HA contents (0, 5, 10 and 20 wt% in relation to the PCL polymer) and evaluated their mechanical properties and in vitro biocompatibility to examine their potential applications in bone tissue engineering. All the prepared scaffolds had a highly aligned porous structure, in which the HA particles were uniformly dispersed in the PCL walls. The elastic modulus of the PCL/HA scaffolds significantly increased from 0.12 ± 0.02 to 2.65 ± 0.05 MPa with increasing initial HA content from 0 to 20 wt%, whereas the pore size decreased from 9.2 ± 0.7 to 4.2 ± 0.8 μm. In addition, the PCL/HA scaffolds showed considerably enhanced in vitro cellular responses that were assessed in terms of cell attachment, proliferation and osteoblastic differentiation.     

Syntheses,magnetic properties,and reactivity of dinuclear oxovanadium (IV) and copper (II) complexes with (μ-diphenylphosphinato)-bridges

Novel dinuclear oxovanadium (IV) complexes having the formula [(VO)₂(dpp)₃(bpy)₂]NO₃·2H₂O (1), [(VO)₂(dpp)₃(phen)₂]-NO₃·H₂O (2), [(VO)₂(bmp)₃(bpy)₂]NO₃·H₂O (3), and [(VO)₂(bmp)₃(phen)₂]NO₃·H₂O (4), and copper (II) complexes having the formula [Cu₂(bmp)₂(phen)₂](NO₃)₂·MeOH·H₂O (5), and [Cu₂(bmp)₂(bpy)₂](NO₃)₂ (6) (where Hdpp=diphenylphosphinic acid, Hbmp=bis(4-methoxyphenyl)phosphinic acid, bpy=2,2^′-bipyridine, and phen=1,10-phenanthroline) with (μ-phosphinato)-bridges, 1–6, have been prepared and characterized. Crystal structure of complex 2 reveals that two vanadium ions are linked by tris(μ-phosphinato)-bridges. The magnetic susceptibility data for 1–3, and 6 conform to the usual dimer equation with −2J values of 16–24 cm⁻¹, indicating a weak antiferromagnetic interaction between vanadium(IV) ions.The oxidation of cinnamyl alcohol was studied using complexes 1–6 as catalyst and molecular oxygen as an oxidant. In the presence of complex 3 as a catalyst, cinnamyl alcohol was oxidized to cinnamaldehyde 61% yield in 7 h. Consequently, complex 3 activates oxygen, and then alcohol was quite efficiently oxidized by activated oxygen.     

Electromagnetic wave reflection loss and magnetic properties of M-type SrFe12−x(Mn0.5Sn0.5)xO19 hexagonal ferrite nanoparticles in the Ku microwave band

Ferrimagnetic nanoparticles of SrFe_12−x(Mn_0.5Sn_0.5)_xO₁₉ was synthesis by controlling the effective processing parameters of sol-gel techniques. Microwave, magnetic properties and structure of nanosize, high purity sol-gel synthesized SrFe_12−x(Mn_0.5Sn_0.5)_xO₁₉ hexaferrite ferrimagnetic nanoparticles were investigated by vector network analysis, vibrating sample magnetometry, EDS and XRD. 57Fe Mössbauer spectroscopy was employed to find the occupancy sites of incorporated cations. The position of manganese and tin in 12k sites caused reduction in coercivity and magnetization saturation. The values of coercivity and magnetization saturation show that superparamagnetism did not occur in the synthesized products. Results demonstrate that additions of manganese and tin to hexagonal ferrite enhance bandwidth and reflection loss. Such composition could be proposed as a suitable electromagnetic wave absorber in microwave frequencies.     

Effect of Nb substitution on magnetic,ferroelectric and photocatalytic properties of Bi0.95Sm0.05Fe1-xNbxO3 (0 ≤ x ≤ 0.1) nanoparticles

The single phase Bi_0.95Sm_0.05Fe_1-xNb_xO₃ (0 ≤ x ≤ 0.1) nanoparticles were synthesized by the sol-gel route, and the effect of Nb substitution on their magnetic, ferroelectric and photocatalytic properties were studied. X-ray diffractometry confirms a phase transformation from rhombohedral to orthorhombic with an increase in Nb substitution. The grain size decreases significantly, and the morphology of grains becomes homogeneous with the increase of Nb concentration. The maximum remnant magnetization (0.014 emu/g), coercivity (565 Oe) and polarization (0.592 μC/cm²) are observed in Bi_0.95Sm_0.05Fe_0.9Nb_0.1O₃. It has been observed that the energy band gap has been slightly reduced from 2.14 to 2.03 eV with Nb substitution, indicating an improvement of photocatalytic activity. The methylene blue degradation is used to represent the photocatalytic ability of Bi_0.95Sm_0.05Fe_1-xNb_xO₃ nanoparticles. The highest degradation efficiency (~74%) of methylene blue is obtained in Bi_0.95Sm_0.05Fe_0.93Nb_0.07O₃, which is much higher than that of Bi_0.95Sm_0.05FeO₃ (~51%) and can be attributed to the optimum particle size and the smallest energy band gap.     

Poly(N-isopropylacrylamide)-coated β-cyclodextrin–capped magnetic mesoporous silica nanoparticles exhibiting thermal and pH dual response for triggered anticancer drug delivery

In this research a novel controlled anticancer drug delivery system with dual pH and thermal responses was designed based on magnetic mesoporous silica nanoparticles that were anchored by β-cyclodextrin and coated by poly(N-isopropylacrylamide) (PNIPAM). Results demonstrated that the behavior of doxorubicin (anticancer drug) release depended on pH and temperature conditions. At endosomal pH (pH 5.5) the amount of drug release enhanced because the cap was removed from the pores. Furthermore, PNIPAM shell collapsed above the lower critical solution temperature and the releasing of drug increased. Thus, this nanocarrier would have the potential to be applied in the tumor therapy.     

pH-Sensitive performance of dextran–poly(acrylic acid) copolymer and its application in controlled in vitro release of ibuprofen

Dextran–poly(acrylic acid) copolymers (D-A) are prepared through copolymerizing of acrylic acid (AA) with dextran. Their structural properties and performances are characterized using various methods. The results indicate that the carboxyl groups of poly(acrylic acid) strongly interact with the proton acceptors of glucose units in dextran, and the effects of AA/dextran molar ratio on the pH sensitivity of obtained copolymers are remarkable. The D-A copolymer shows a smart pH response, specifically, shrinkage in a low pH medium and swelling at high pH. The potential application of D-A copolymer as a drug delivery matrix is explored using ibuprofen as a model drug.     

Synthesis,crystal structure and magnetic properties of a new 2D cyanide-bridged heterobimetallic Cr(I)–Mn(III) complex

A new two-dimensional cyanide-bridged Cr(I)–Mn(III) coordination polymer {K[Mn(L)]₂[Cr(CN)₅NO]}·CH₃CN (1) (L = N,N-ethylene-bis(3-methoxysalicylideneiminate)) has been successfully synthesized by the reaction of K₃[Cr(CN)₅NO] with [Mn(L)(H₂O)₂]ClO₄ and characterized by elemental analysis, FT-IR and X-ray structure determination. Investigation systematic over magnetic susceptibility of the complex reveals the overall antiferromagnetic interaction between the cyanide-bridged Cr(I) ion and Mn(III) ion and its 3D antiferromagnetic ordering behavior with typical metamagnetic character below 12.5 K.     

Poly(DL-lactide-co-ε-caprolactone) and poly(DL-lactide-co-glycolide) blends for biomedical application: Physical properties,cell compatibility,and in vitro degradation behavior

Poly(DL-lactide-co-ε-caprolactone) (PLCL) and poly(DL-lactide-co-glycolide) (PLGA) blends of various compositions were prepared. Fractured sections of PLCL/PLGA blends did not evidence phase separation and blend glass transition temperatures suggested some degree of blend compatibility. The elastic modulus showed a negative deviation from the additive law of mixture. Superior biocompatibility in terms of fibroblast NIH 3T3 cell adhesion and proliferation, better mechanical properties, and a more homogeneous phase were obtained with PLCL/PLGA 25/75 blend. Rapid degradation of PLCL phase (4–8 weeks) in PLCL/PLGA 25/75 blend led to a porous structure, which makes it a potential candidate for drug delivery systems.     

Structural,magnetic and magnetocaloric properties of CoFe2−xMoxO4 (0.0≤x≤0.3) ferrites

We have investigated structural, magnetic and magnetocaloric properties of CoFe_2-xMo_xO₄ (0.0≤x≤0.3) ferrites. Polycrystalline samples were prepared by the sol gel method and characterized by the powder X-ray diffraction and scanning electron microscopy. X-ray diffraction patterns show that all samples have a cubic spinel structure and the lattice parameter, a, decreases monotonically with increase in Mo concentration. Scanning electron micrographs indicate that most of the particles are in the range of 400–850 nm size. Magnetic measurements, performed by using a cryogen free vibrating sample magnetometer, show that these samples are soft ferromagnets in the measured temperature range. The saturation magnetization, M_s, values of Mo-doped samples are larger than the parent compound with a maximum value of ~106 emu/g for x=0.2 sample. The magnetic entropy change (−ΔS) increases with increase in applied magnetic field and shows a peak in the vicinity of blocking temperature. A maximum value of 0.56 J kg⁻¹ K⁻¹ at 5 T field has been observed for x=0.2 sample.