Microstructures, mechanical behavior, cellular response, and hemocompatibility of bulk ultrafine-grained pure tantalum.

Bulk ultrafine-grained (UFG) pure Ta had been successfully prepared by equal channel angular pressing (ECAP) technique till eight passes. The 1st, 2nd, 4th, and 8th ECAPed Ta samples were investigated in the current study, with the 0th ECAPed Ta sample as the microcrystalline counterpart control. The microstructure and grain size distribution were characterized by X-ray diffractometer patterns, scanning electron microscopy, and transmission electron microscopy analysis by means of histogram. Although the mechanical behavior of all the experimental samples were analyzed through uniaxial tensile measurement and microhardness test, in vitro biological interactions onto the substrates such as protein adsorption, cellular responses derived from different types of cell lines, and the activity of erythrocyte and platelets were further evaluated and specifically assessed by bicinchoninic acid assay, enzyme-linked immunosorbent assay, and the method of colorimetric reading. A superior percentage of protein adsorption can be observed on the substrate of the UFG 8th ECAPed Ta (around 90%), even above those on the tissue culture plate (control) and the other ECAPed Ta samples. Furthermore, the UFG 8th ECAPed Ta shows no cytotoxic within 4 days culture when incubated with the murine fibroblast cell lines (L929). In addition, a priority order in the growth of endothelial cells (ECV304) other than vascular smooth muscle cells was observed in the case of the UFG 8th ECAPed Ta. In terms of hemolysis rate and adhered platelets (both the amount and the individual morphology), an evolutionary outcome of preferentially enhanced hemocompatibility can be concluded for the case of the UFG 8th ECAPed Ta.

In vitro and in vivo studies on nanocrystalline Ti fabricated by equal channel angular pressing with microcrystalline CP Ti as control.

Bulk nanocrystalline Ti bars (Grade 4, Φ4 × 3000 mm(3)) were massively fabricated by equal channel angular pressing (ECAP) via follow-up conform scheme with the microcrystalline CP Ti as raw material. Homogeneous nanostructured crystals with the average grain size of 250 nm were identified for the ECAPed Ti, with extremely high tensile/fatigue strength (around 1240/620 MPa) and adorable elongation (more than 5%). Pronounced formation of bonelike apatite for the nanocrystalline Ti group after 14 days static immersion in simulated body fluids (SBF) reveals the prospective in vitro bioactive capability of fast calcification, whereas an estimated 17% increment in protein adsorption represents good bioaffinity of nanocrystalline Ti. The documentation onto the whole life circle of osteoblast cell lines (MG63) revealed the strong interactions and superior cellular functionalization when they are co-incubated with bulk nanocrystalline Ti sample. Moreover, thread-structured specimens were designed and implanted into the tibia of Beagles dogs till 12 weeks to study the in vivo responses between bone and metallic implant made of bulk nanocrystalline Ti, with the microcrystalline Ti as control. For the implanted nanostructured Ti group, neoformed bone around the implants underwent the whole-stage transformation proceeding from originally osteons or immature woven bone to mature lamellar bone (skeletonic trabecular), even with the remodeling being finished till 12 weeks. The phenomenal osseointegration of direct implant-bone contact can be revealed from the group of the ECAPed Ti without fibrous tissue encapsulation in the gap between the implant and autogenous bone.

Surface chemistry of bulk nanocrystalline pure iron and electrochemistry study in gas-flow physiological saline.

Conventional microcrystalline pure iron (MC-Fe) becomes a new candidate as biodegradable metals, which has the insufficient physical feature and inferior biodegradation behavior. Novel bulk nanocrystalline pure iron (NC-Fe) was fabricated via equal channel angular pressing technique in the present work to overcome these problems. The contact angle test with water and glycerol droplets shows a smaller angle (though >90°) of NC-Fe than that of MC-Fe, which implies a lower surface energy of NC-Fe. The surface roughness of NC-Fe increased greatly than that of MC-Fe. A further comparative study of corrosion and electrochemistry performance between NC-Fe and its original MC-Fe was investigated in physiological saline with different dissolved oxygen concentration, aiming to in vitro simulate the corrosion process of coronary stent occurred in physiological environment. The electrochemical impedance spectra analysis and anodic polarization measurements indicated that the NC-Fe exhibited higher corrosion resistance than that of the MC-Fe; meanwhile obvious enhanced corrosion resistance with the decrement of dissolved oxygen concentration was observed. Related equivalent circuit model and surface reconstruction process were further discussed, and the degradation mechanism of the MC-Fe and NC-Fe were finally established.

Effective inhibition of the early copper ion burst release with ultra-fine grained copper and single crystal copper for intrauterine device application.

To solve the main problems of existing coarse grained copper (CG Cu) intrauterine devices (IUD)-namely burst release and a low transfer efficiency of the cupric ions during usage-ultra-fine grained copper (UFG Cu) and single crystal copper (SC Cu) have been investigated as potential substitutes. Their corrosion properties with CG Cu as a control have been studied in simulated uterine fluid (SUF) under different conditions using electrochemical measurement methods. Long-term immersion of UFG Cu, SC Cu and CG Cu samples in SUF at 37 °C have been studied for 300 days. A lower copper ion burst release and a higher efficiency release of cupric ions were observed for UFG Cu and SC Cu compared with CG Cu in the first month of immersion and 2 months later. The respective corrosion mechanisms for UFG Cu, SC Cu and CG Cu in SUF are proposed. In vitro biocompatibility tests show a better cellular response to UFG Cu and SC Cu than CG Cu. In terms of instantaneous corrosion behavior, long-term corrosion performance and in vitro biocompatibility, the three pure copper materials follow the order: UFG Cu>SC Cu>CG Cu, which indicates that UFG Cu could be the most suitable candidate material for intrauterine devices.

Comparative study on corrosion resistance and in vitro biocompatibility of bulk nanocrystalline and microcrystalline biomedical 304 stainless steel.

OBJECTIVES: SUS 304 stainless steels have been widely used in orthodontics and implants such as archwires, brackets, and screws. The purpose of present study was to investigate the biocompatibility of both the commercial microcrystalline biomedical 304 stainless steel (microcrystalline 304ss) and novel-fabricated nanocrystalline 304 stainless steel (nanocrystalline 304ss). METHODS: Bulk nanocrystalline 304ss sheets had been successfully prepared by microcrystalline 304ss plates using severe rolling technique. The electrochemical corrosion and ion release behavior immersion in artificial saliva were measured to evaluate the property of biocorrosion in oral environment. The cell lines of murine and human cell lines from oral and endothelial environment were co-cultured with extracts to evaluate the cytotoxicity and provide referential evidence in vivo. RESULTS: The polarization resistance trials indicated that nanocrystalline 304ss is more corrosion resistant than the microcrystalline 304ss in oral-like environment with higher corrosion potential, and the amount of toxic ions released into solution after immersion is lower than that of the microcrystalline 304ss and the daily dietary intake level. The cytotoxicity results also elucidated that nanocrystalline 304ss is biologically compatible in vitro, even better than that of microcrystalline 304ss. SIGNIFICANCE: Based on the much higher mechanical and physical performances, nanocrystalline 304ss with enhanced biocorrosion property, well-behaved in vitro cytocompatibility can be a promising alternative in orthodontics and fixation fields in oral cavity.

In vitro corrosion, cytotoxicity and hemocompatibility of bulk nanocrystalline pure iron.

Bulk nanocrystalline pure iron rods were fabricated by the equal channel angular pressure (ECAP) technique up to eight passes. The microstructure and grain size distribution, natural immersion and electrochemical corrosion in simulated body fluid, cellular responses and hemocompatibility were investigated in this study. The results indicate that nanocrystalline pure iron after severe plastic deformation (SPD) would sustain durable span duration and exhibit much stronger corrosion resistance than that of the microcrystalline pure iron. The interaction of different cell lines reveals that the nanocrystalline pure iron stimulates better proliferation of fibroblast cells and preferable promotion of endothelialization, while inhibits effectively the viability of vascular smooth muscle cells (VSMCs). The burst of red cells and adhesion of the platelets were also substantially suppressed on contact with the nanocrystalline pure iron in blood circulation. A clear size-dependent behavior from the grain nature deduced by the gradual refinement microstructures was given and well-behaved in vitro biocompatibility of nanocrystalline pure iron was concluded.