Comparison of conventional and severe shot peening effects on the microstructure, texture, roughness, hardness, and electrochemical behavior of austenitic stainless steel.

In the present research, microstructure, texture, roughness, hardness, and electrochemical behavior of AISI 316L austenitic stainless steel before and after shot peening were studied to elucidate the effect of conventional and severe shot peening (CSP and SSP) processes. After the shot peening, the fraction of strain-induced martensite (SIM) and mechanical twins (MTs) in the sub-surface layer was increased. The fraction of SIM and MTs in the SSP sample was higher than in the CSP sample. The XRD patterns indicated that the SSP sample had a higher peak broadening compared to the CSP sample. In the CSP and SSP samples, a gradient microstructure was formed along the depth direction. The microstructure of the topmost layer of the CSP and SSP samples exhibited numerous ultrafine grains. The grain refining during severe shot peening was faster because of the accumulation of more strain. The CSP and SSP samples revealed a gradient distribution of elements. After the SSP, the intensity of ⟨110⟩‖ED fiber texture decreased from 12.7 to 11.6 × R and the average intensity of ⟨100⟩‖ED fiber texture increased from 1.7 to 2.0 × R, respectively, compared to the CSP sample. The surface roughness of the SSP sample (Rq = 73.6 nm and Ra = 45.2 nm) was lower than that of the CSP sample which represented the roughness decreased with surface coverage increasing from 100 % to 1500 %. Also, the wettability increased after the conventional and severe shot peening processes. In addition, the microhardness of the CSP and SSP samples showed a gradient distribution. The CSP sample had the lowest corrosion current density (0.13 µA/cm2) whereas the NP (non-peened) sample exhibited the highest current density (0.65 µA/cm2). The presence of ⟨100⟩-oriented grains in both CSP and SSP samples led to the higher corrosion resistance of shot-peened steels compared to the NP sample. The presence of favorable texture with higher intensity in the CSP sample was responsible for the higher corrosion resistance of the CSP sample compared to the SSP sample. Finally, the gradient distribution of elements along the depth direction in the CSP and SSP steels improved the corrosion resistance of the surface.

Synthesis and characterization of mupirocin-LDH/PVA nanofibrous composite as a dual-carrier drug release system.

Nowadays, nanofibrous structures based on organic and inorganic materials are considered a drug delivery system for the controlled release of antibiotics and other antibacterial agents. The main goal of this research is a combination of the special properties of nanofibrous structure and Mupirocin-loaded Layered double hydroxide (LDH) to obtain a dual-carrier drug release system to provide long term antibacterial properties in wound healing process. Regards, unloaded layered double hydroxide (LDH) and Mupirocin-loaded LDH, which were synthesized by co-precipitation method, were added to Polyvinyl alcohol (PVA) solution in different mass ratio and electrospun using different processing conditions. The physico-chemical characterizations were performed using SEM, FTIR and tensile strength tests. The biological properties of the fabricated nanocomposites were evaluated using antibacterial test and in vitro cell culturing followed by MTT assay. The SEM results showed a bead-less and uniform morphology of nanofibrous composite containing Mupirocin(2.3 wt%)-LDH(15 wt%)/PVA with an average fiber diameter of about 270 ± 58 nm. According to the release study, the maximum release of the mupirocin drug was about 54 % in the first 6 h. The antibiogram analysis exhibited good antibacterial activity of mupirocin-loaded nanocomposite against both bacteria, especially gram-positive one. Finally, MTT assay approved the biocompatibility of the mupirocin-loaded nanocomposite. Overall, the produced nanofibrous composites would be a promising dual-carrier system for controlled release of antibiotic.

Fabrication of a gradient AZ91-bioactive glass composite with good biodegradability.

This study used friction stir-back extrusion to fabricate the AZ91 + 3 wt% bioactive glass gradient composite wire. The microstructure, mechanical properties, and corrosion resistance of a material in a simulated body fluid were investigated. Three 2-mm diameter holes with varying hole patterns were drilled in the cross-section of the AZ91 rod to apply 3 wt % bioactive glass to the AZ91 matrix. The results demonstrated that the hole pattern strongly influenced the material's flow in the extruded wire's cross-section. By increasing the distance between the center of the initial rod and the center of the holes, a higher temperature and more uniform distribution of plastic strain are formed during friction stir back extrusion, resulting in uniform distribution of bioactive glass particles and α + ß eutectic structure near the surface of composite wires. Introducing bioactive glass particles into the zone near the surface of the AZ91 rod results in the formation of a uniform distribution of bioactive glass particles near the surface and their absence in the central zone of the composite wire. A higher amount of discontinuous ß-Mg17Al12 phase and α + ß eutectic formed at the grain boundaries by increasing the temperature and plastic strain during friction stir-back extrusion. The crystallographic texture of the AZ91 rod changed from prismatic to basal and pyramidal due to the friction stir-back extrusion method. A gradient AZ91-bioactive glass composite wire with ultimate tensile strength, yield strength, elongation, and corrosion resistance 58, 64, 62, and 34%, respectively, greater than AZ91 as-cat rod can be produced by inserting bioactive glass powder using a hole drilling method and applying a friction stir back extrusion process.

Synthesis and characterization of a calcium phosphate bone cement with quercetin-containing PEEK/PLGA microparticles.

This study aimed to describe the synthesis and characterization of a calcium phosphate cement (CPC) with polyetheretherketone/poly (lactic-co-glycolic) acid (PEEK/PLGA) micro-particles containing quercetin. CPC powder was synthesized by mixing dicalcium phosphate anhydrate and tetracalcium phosphate. To synthesize PEEK/PLGA microparticles, PLGA85:15 was mixed with 90 wt% PEEK. The weight ratio of quercetin/PLGA/PEEK was 1:9:90 wt%. PEEK/PLGA/quercetin microparticles with 3, 5, and 6 wt% was added to CPC. The setting time, compressive strength, drug release profile, solubility, pH, and porosity of synthesized cement were evaluated. The morphology and physicochemical properties of particles was analyzed by scanning electron microscopy, Fourier-transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), and inductively coupled plasma. Cytotoxicity was assessed by the methyl thiazolyl tetrazolium assay using dental pulp stem cells. Expression of osteoblastic differentiation genes was evaluated by real-time polymerase chain reaction. Data were analyzed by one-way ANOVA and Tukey's test (alpha = 0.05). The setting time of 3 wt% CPC was significantly longer than 5 and 6 wt% CPC (P< 0.001). The 6 wt% CPC had significantly higher compressive strength than other groups (P= 0.001). The release of quercetin from CPCs increased for 5 d, and then reached a plateau. XRD and FTIR confirmed the presence of hydroxyapatite in cement composition. Significantly higher expression of osteocalcin (OCN) and osteopontin (OPN) was noted in 3 wt% and 6 wt% CPCs. Addition of quercetin-containing PEEK/PLGA microparticles to CPC enhanced its compressive strength, decreased its setting time, enabled controlled drug release, and up-regulated OPN and OCN.

Biological and bioactivity assessment of dextran nanocomposite hydrogel for bone regeneration.

Insufficient biological and bioactive properties of dextran hydrogels limit their applications as promising scaffolds for tissue engineering. We developed nanocomposite dextran hydrogels comprised of bioactive glass (nBGC: 64% SiO2, 31% CaO, 5% P2O5) nanoparticles with an average particle size of 77 nm using a chemical crosslinking of dextran chains to form 3D hydrogel networks. In the current study; bioactivity of the obtained nanocomposite hydrogels was evaluated through the formation of apatite crystal structures after the incubation in simulated body fluid (SBF) at various submersion periods and nBGC content. The scanning electron microscopy (SEM) micrographs represented an enhanced hydroxyapatite formation on the cross section of nanocomposite comprising of nBGC content from 2 to 8 (% by wt). Biomineralization results of Dex-8 (% by wt) composite during 7, 14 and 28 days immersion indicated the apatite layer formation and the growth of apatite crystal size on the surface and cross section of the nanocomposite. Moreover, MTT assessments indicated that human osteosarcoma cells (SaOS-2) were able to adhere and spread within the dextran hydrogels reinforced with the bioactive glass nanoparticles. With regard to enhanced bioactivity and biocompatibility, the developed dextran-nBGC hydrogel could be considered as a suitable candidate for bone tissue engineering application.

Fabrication and physicochemical characterization of a novel magnetic nanocomposite scaffold: Electromagnetic field effect on biological properties.

In the current research, a novel poly(ε-caprolactone) nanofibrous composite scaffold including CZF-NPs1 (cobalt­zinc ferrite nanoparticles) was investigated to study the physical, mechanical and biological properties of new magnetic nanofibrous materials and then to evaluate the effect of applied electromagnetic field on biological properties of these scaffolds. It was observed that the incorporation of CZF-NPs up to 3 wt.% leads to decrease in nanofibers' diameter to 466 nm. By raising the content of CZF-NPs, hydrophilicity and biodegradation of magnetic nanofibrous scaffolds improved significantly. In addition, the mechanical properties of nanofibers such as stress at break point was interestingly increased in the sample with 3 wt.% of CZF-NPs. The results of biocompatibility, cell adhesion and cell staining assays with L929 cells are much more improved in nanofibers embedded with CZF-NPs in the presence of external electromagnetic field (EMF). According to this study, magnetic nanofibrous scaffolds composed of PCL/CZF-NPs could be considered as a promising candidate to regenerate damaged tissues.

Novel calcium phosphate coated calcium silicate-based cement: in vitro evaluation.

Calcium silicate-based cements are known for their wide applications in dentistry and orthopedics. The alkaline pH (up to 12) of these cements limits their application in other orthopedic areas. In this study, the effect of dicalcium phosphate dihydrate (DCPD) coating on set cement on pH reduction and biocompatibility improvement was examined. Samples with 0 and 10 weight ratio DCPD were prepared and characterized by XRD, FTIR, and SEM. The DCPD coating on the set cement was performed by a 7 d immersion in 1% monocalcium phosphate (MCP) solution and characterized by XRD, FTIR, SEM, and EDX. Also, the compressive strength and cytotoxicity of the samples were tested. The results showed that DCPD coating did not significantly change the compressive strength of the cement, but by decreasing the pH of the culture medium to the physiological range, it led to enhance adhesion, spreading and proliferation of human osteosarcoma cell line (Saos-2). The novel DCPD coated calcium silicate-based cement could be served as a bulk or porous bone substitute and scaffold.

Fabrication and characterization of dextran/nanocrystalline ß-tricalcium phosphate nanocomposite hydrogel scaffolds.

Design of bioactive three-dimensional scaffolds to support bone tissue repair and regeneration become a key area of research in tissue engineering. Herein, porous hybrid hydrogels composed of dextran incorporated with nanocrystalline ß-tricalcium phosphate (ß-TCP) particles were tailor made as scaffolds for bone tissue engineering. ß-TCP was successfully introduced within the dextran networks crosslinked through intermolecular ionic interactions and hydrogen bonding confirmed by FTIR spectroscopy. The effect of ß-TCP content on equilibrium water uptake and swelling kinetics of composite hydrogels was investigated. It was found that the homogeneous distribution of ß-TCP nanoparticles through the hydrogel matrix contributes to higher porosity and swelling capacity. In depth swelling measurements revealed that while in the early stage of swelling, water diffusion follows the Fick's law, for longer time swelling behavior of hydrogels undergo the second order kinetics. XRD measurements represented the formation of apatite layer on the surface of nanocomposite hydrogels after immersion in the SBF solution, which implies their bioactivity. Cell culture assays confirmed biocompatibility of the developed hybrid hydrogels in vitro. The obtained results converge to offer dextran/ß-TCP nanocomposite hydrogels as promising scaffolds for bone regeneration applications.

Electrospun Poly-ε-Caprolactone (PCL)/Dicalcium Phosphate Dihydrate (DCPD) Composite Scaffold for Tissue Engineering Application.

Recently electrospun scaffolds show excellent response in cell adhesion, growth, and tissue healing in comparison with other techniques. So in this study, PCL and PCL/DCPD scaffolds were designed and prepared with electrospinning. The electrospun scaffolds were characterized by scanning electron microscope with X-ray elemental analysis, atomic force microcopy, differential scanning calorimetry, and contact angle analysis for optimizing the effective parameters. Fiber formation with uniform diameter and bead-free structure was obtained. Scaffold surface roughness increased from 100 nm for PCL to 440 nm for PCL/DCPD. DSC analysis showed the effects of DCPD on thermal stability of composite scaffold and the results of contact angle evaluation indicate improved hydrophilicity and ability of water absorption of PCL/DCPD composite fibers as compared to PCL fibers. MTT assay indicated lack of toxicity for human gingival fibroblast (HGF) cells after cell seeding on scaffold. Also, the composite scaffold can improve cell viability by helping their growth on its surface. So it can be concluded that by engineering the electrospinning parameters we can fabricate a PCL/DCPD composite scaffold for tissue engineering applications.

Nanostructured akermanite glass-ceramic coating on Ti6Al4V for orthopedic applications.

Glass ceramics are widely used to enhance the functionality of inert metallic materials typically used for hard-tissue engineering. Biofunctionality of glass ceramics can in turn be significantly boosted with the addition of trace element dopants. Herein, we synthesized a nanostructured glass ceramic and used magnesium (Mg), which is known to promote osteoblast adhesion and proliferation, for further functionalization. The nanostructured akermanite glass ceramic (Ca2MgSi2O7) was used to coat Ti6Al4V substrates by the sol-gel method. Scanning and transmission electron microscopy as well as X-ray diffraction were used to assess the structural morphology and phase composition of the coating, respectively. The micrographs showed a uniform and crack-free coating structure. Atomic force microscopy observation revealed a disordered surface roughness for coated samples. In vitro cytocompatibility tests revealed that Saos-2 cells cultured on bare samples adopted a rounded morphology, whereas cells cultured on the coated samples represented a more spread out configuration and also increased proliferation. The characterizing tests confirmed the efficiency of the synthesis method and the in vitro biocompatibility of the synthesized coating, indicating its suitability to be used for bone implants.

Dextran hydrogels incorporated with bioactive glass-ceramic: Nanocomposite scaffolds for bone tissue engineering.

A series of nanocomposite scaffolds comprised of dextran (Dex) and sol-gel derived bioactive glass ceramic nanoparticles (nBGC: 0-16 (wt%)) were fabricated as bioactive scaffolds for bone tissue engineering. Scanning electron microscopy showed Dex/nBGC scaffolds were consisting of a porous 3D microstructure with an average pore size of 240 µm. Energy-dispersive x-ray spectroscopy illustrated nBGC nanoparticles were homogenously distributed within the Dex matrix at low nBGC content (2 wt%), while agglomeration was observed at higher nBGC contents. It was found that the osmotic pressure and nBGC agglomeration at higher nBGC contents leads to increased water uptake, then reduction of the compressive modulus. Bioactivity of Dex/nBGC scaffolds was validated through apatite formation after submersion in the simulated body fluid. Dex/nBGC composite scaffolds were found to show improved human osteoblasts (HOBs) proliferation and alkaline phosphatase (ALP) activity with increasing nBGC content up to 16 (wt%) over two weeks. Owing to favorable physicochemical and bioactivity properties, the Dex/nBGC composite hydrogels can be offered as promising bioactive scaffolds for bone tissue engineering applications.

Synergic effect of chitosan and dicalcium phosphate on tricalcium silicate-based nanocomposite for root-end dental application.

In recent years, cement composites based on calcium silicate have been more generally considered for medical applications. Calcium silicate Cement are among the categories that are used in dental root canal treatment. The aim of this study is to make new calcium silicate cement with dicalcium phosphate and chitosan additives to preserve and strengthen desirable properties of this type of cements. In this study, composite dental cement based on calcium silicate was prepared. Then effect of adding biodegradable and biocompatible polymer such as chitosan on setting properties and its structure were studied. In this study, a combination of calcium silicate, dicalcium phosphate (DCP) and bismuth oxide (Bi2O3) as powder phase and 2% solution of the chitosan dissolved in 1% acetic acid solution as liquid phase, was used. As well as control sample was obtained by mixing the powder with distilled water as the liquid phase. Based on the obtained results, setting time of composite cement was changed from 51 to 67 minutes by adding chitosan polymer. Presence of chitosan also reduced the compressive strength a little. The bioactivity of the cement were studied in a solution of simulated body fluid (SBF) for 14 days. The samples were analyzed by SEM to identify the microstructure and by XRD to determine crystal structure. The composition of cement before incubation in SBF was included early phases (phase calcium silicate and calcium phosphate) that after 14 days of immersion in SBF, they were converted to layer-shaped hydroxy apatite and the presence of chitosan had not any influence on the final phase of hydroxy apatite.

Effect of CO2 laser power intensity on the surface morphology and friction behavior of alumina ceramic brackets.

OBJECTIVE: This study aims at reducing frictional resistance of the ceramic brackets by using CO2 laser irradiation. METHODS: Forty-two polycrystalline Al2 O3 ceramic brackets were randomly divided into six groups of seven samples: a control group B0 (not subjected to laser irradiation) and five groups subjected to irradiation with intensities of 10 (B10), 30 (B30), 70 (B70), 90 (B90), and 110 (B110) J/cm2 . After irradiation, two samples from each group were evaluated by scanning electron microscopy (SEM) and atomic force microscopy (AFM), while the remaining five samples were tested for frictional resistance. The sliding friction of stainless steel wires (SS-wires) in the brackets was measured using a universal testing machine. RESULTS: Samples from the first set (groups B0, B10, and B30) were significantly more resistant to wire sliding than the samples from the second set (groups B70, B90, and B110). The SEM analysis shows different degrees of blister formation on the bracket surfaces subjected to laser irradiation and no changes in their grain sizes. The AFM results indicate more consistent blister formation for groups B70, B90, and B110 than for other groups. CONCLUSION: Different CO2 laser power intensities significantly affect frictional resistances of SS-wires in Al2 O3 ceramic brackets.

Antimicrobial effect, frictional resistance, and surface roughness of stainless steel orthodontic brackets coated with nanofilms of silver and titanium oxide: a preliminary study.

Nano-silver and nano-titanium oxide films can be coated over brackets in order to reduce bacterial aggregation and friction. However, their antimicrobial efficacy, surface roughness, and frictional resistance are not assessed before. Fifty-five stainless-steel brackets were divided into 5 groups of 11 brackets each: uncoated brackets, brackets coated with 60 µm silver, 100 µm silver, 60 µm titanium, and 100 µm titanium. Coating was performed using physical vapor deposition method. For friction test, three brackets from each group were randomly selected and tested. For scanning electron microscopy and atomic-force microscopy assessments, one and one brackets were selected from each group. For antibacterial assessment, six brackets were selected from each group. Of them, three were immediately subjected to direct contact with S. mutans. Colonies were counted 3, 6, 24, and 48 h of contact. The other three were stored in water for 3 months. Then were subjected to a similar direct contact test. Results pertaining to both subgroups were combined. Groups were compared statistically. Mean (SD) friction values of the groups 'control, silver-60, silver-100, titanium-60, and titanium-100' were 0.55 ± 0.14, 0.77 ± 0.08, 0.82 ± 0.11, 1.52 ± 0.24, and 1.57 ± 0.41 N, respectively (p = .0004, Kruskal-Wallis). Titanium frictions were significantly greater than control (p < .05), but silver groups were not (p > .05, Dunn). In the uncoated group, colony count increased exponentially within 48 h. The coated groups showed significant reductions in colony count (p < .05, two-way-repeated-measures ANOVA). In conclusions, all four explained coatings reduce surface roughness and bacterial growth. Nano-titanium films are not suitable for friction reduction. Nano-silver results were not conclusive and need future larger studies.

Development and characterization of a bioglass/chitosan composite as an injectable bone substitute.

SiO2-CaO-P2O5 based bioglass (BG) systems constitute a group of materials that have wide applications in bone implants. Chitosan (Cn) is a biocompatible and osteoconductive natural polymer that can promote wound healing. In this study, bioactivity of chitosan/bioglass (CnB) composites as minimally invasive bone regenerative materials was assessed both in vitro and in vivo. Injectability tests and scanning electron microscopy (SEM) results demonstrated the formation of uniform injectable paste-like composites using BG particles and Cn. Fourier transform infrared spectroscopy (FTIR) and SEM images confirmed hydroxyapatite deposition in vitro after incubation in simulated body fluid (SBF). Higher BG content in the composite correlated with increased human osteoblast proliferation. An in vivo study in a rat spinal fusion model confirmed that increasing the amount of BG improved osteoconductivity. Manual palpation, radiographic images and pathological assessments proved that the composites promote bone formation. Based on these data, the synthesized composites have a potential application in orthopedic and reconstructive surgeries as a minimally invasive bone substitute.

Evaluation of Antibacterial Effects of Silver-Coated Stainless Steel Orthodontic Brackets.

OBJECTIVES: White spots and enamel demineralization around orthodontic brackets are among the most important complications resulting from orthodontic treatments. Since the antibacterial properties of metals and metallic particles have been well documented, the aim of this study was to assess the antibacterial effect of stainless steel orthodontic brackets coated with silver (Ag) particles. MATERIALS AND METHODS: In this study, 40 standard metal brackets were divided into two groups of 20 cases and 20 controls. The brackets in the case group were coated with Ag particles using an electroplating method. Atomic force microscopy and scanning electron microscopy were used to assess the adequacy of the coating process. In addition, antibacterial tests, i.e., disk diffusion and direct contact tests were performed at three, six, 24, and 48 hours, and 15 and 30 days using a Streptococcus mutans strain. The results were analyzed using Student's t-test and repeated measures ANOVA. RESULTS: Analyses via SEM and AFM confirmed that excellent coatings were obtained by using an electroplating method. The groups exhibited similar behavior when subjected to the disk diffusion test in the agar medium. However, the bacterial counts of the Ag-coated brackets were, in general, significantly lower (P<0.001) than those of their non-coated counterparts. CONCLUSIONS: Brackets coated with Ag, via an electroplating method, exhibited antibacterial properties when placed in direct contact with Streptococcus mutans. This antibacterial effect persisted for 30 days after contact with the bacteria.

The effects of silver coating on friction coefficient and shear bond strength of steel orthodontic brackets.

Aims of the present study was to measure frictional resistance between silver coated brackets and different types of arch wires, and shear bond strength of these brackets to the tooth. In an experimental clinical research 28 orthodontic brackets (standard, 22 slots) were coated with silver ions using electroplate method. Six brackets (coated: 3, uncoated: 3) were evaluated with Scanning Electron Microscopy and Atomic Force Microscopy. The amount of friction in 15 coated brackets was measured with three different kinds of arch wires (0.019 × 0.025-in stainless steel [SS], 0.018-in stainless steel [SS], 0.018-in Nickel-Titanium [Ni-Ti]) and compared with 15 uncoated steel brackets. In addition, shear bond strength values were compared between 10 brackets with silver coating and 10 regular brackets. Universal testing machine was used to measure shear bond strength and the amount of friction between the wires and brackets. SPSS 18 was used for data analysis with t-test. SEM and AFM results showed deposition of a uniform layer of silver, measuring 8-10 µm in thickness on bracket surfaces. Silver coating led to higher frictional forces in all the three types of arch wires, which was statistically significant in 0.019 × 0.025-in SS and 0.018-in Ni-Ti, but it did not change the shear bond strength significantly. Silver coating with electroplating method did not affect the bond strength of the bracket to enamel; in addition, it was not an effective method for decreasing friction in sliding mechanics.

Effect of alumina on microstructure and compressive strength of a porous silicated hydroxyapatite.

PURPOSE: We investigated the effects of alumina addition on microstructure and compressive strength of a porous silicate substituted hydroxyapatite (Si-HA). METHODS: Hydroxyapatite (HA) was synthesized under precipitation conditions and 10 %Wt. of sol-gel derived CaO.P2O5.SiO2 based bioglass (BG) powder was added to HA. Polyurethane foam was used to form a high porous structure with integral porosity of 70%. Phase analysis was performed using XRD and FTIR and the microstructure was studied using SEM. RESULTS: The results confirmed that the Si-HA was the only formed phase before Al2O3 addition while after addition the presence of silicon-incorporated HA and alumina without any other phases was proved using these analyses. CONCLUSIONS: The porous structures of Si-HA and Al2O3 were synthesized using the replication technique. The compressive strength of porous bioceramics increased with increasing Al2O3 content up to 30 wt% (ANOVA, P<.05).

The fabrication of nanocomposites via calcium phosphate formation on gelatin-chitosan network and the gelatin influence on the properties of biphasic composites.

A novel biodegradable polymer-ceramic nanocomposite which consisted of gelatin (Gel), chitosan (CS), and calcium phosphate (CaP) nanoparticles was prepared based on in situ preparation method. The fabricated biocomposites were characterized by FTIR, X-ray diffraction (XRD), transmission electron microscopy (TEM) as well as scanning electron microscope with X-ray elemental analysis (SEM-EDX). The characterization results confirmed that the crystalline calcium phosphate nanoparticles were mineralized in polymeric matrix and the interaction between Ca2+ in calcium phosphate and functional groups in polymers molecular chains was formed. XRD result showed that in addition to hydroxyapatite (HA), Brushite (BR) and tricalcium phosphate (ß-TCP) particles also were formed due to lack of complete penetration of the basic solution into the polymeric matrix. However, SEM image indicated that the polymeric matrix has the controlling role in the particle size of calcium phosphate. The size of particles in three component composites was about 100nm while in two component composites proved to be more in µm size. TEM observation supported SEM results and showed that the three component composites have calcium phosphate nanoparticles. The elastic modulus and compressive strength of the composites were also improved by the employment of gelatin and chitosan together, which can make them more beneficial for surgical applications.

Hydroxyapatite scaffolds infiltrated with thermally crosslinked polycaprolactone fumarate and polycaprolactone itaconate.

In this work, two unsaturated derivatives of polycaprolactone (PCL), polycaprolactone fumarate (PCLF), and polycaprolactone itaconate (PCLI), have been synthesized and used as an infiltrating polymer to improve the mechanical properties of brittle hydroxyapatite (HA) scaffolds. PCLF and PCLI were first synthesized through polyesterification of the low molecular weight PCL diols with fumaryl chloride and itaconyl chloride respectively, and then characterized by Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, gel permeation chromatography, and differential scanning calorimetry analysis. HA scaffolds were sintered using a foam replication technique, with porosity of about 60%. Polymer-HA composites were obtained by infiltrating the HA scaffolds with PCLF and PCLI solution (12.5 and 30 w/v in dichloromethane) followed by thermal crosslinking. The polymer infiltrated HA scaffolds were characterized by scanning electron microscopy, porosimetry, and gravimetrical analysis. The polyesterification reaction of PCL diols with fumarate chloride was more efficient than itaconyl chloride and dependent upon the molecular weight of the initial PCL precursor; the resultant PCLF demonstrated a degree of substitution of 1.2, 4.2, and 2.7 times higher than PCLIs. Polymer infiltration improved the compressive strength of the HA scaffolds, and based upon the type of macromer (PCLF or PCLI) and also their concentration in infiltrating solution (12.5 or 30 w/v %) compressive strength increased about 14-328%. In all studied samples, the reinforcement effect of PCLF infiltration was higher than PCLI. The macromers and their corresponding infiltrated HA scaffolds did not show any significant cytotoxicity toward human primary osteogenic sarcoma cell (G92 cell lines), in vitro.