The measurement of cutting force is an effective method for machining condition monitoring in intelligent manufacturing. Titanium nitride films and silicon nitride films were prepared on 304 stainless steel substrates by DC-reactive magnetron sputtering and plasma-enhanced chemical vapor deposition (PECVD). The effects of substrate negative bias and nitrogen flow on the surface microstructures of TiN film were investigated. The smoothness of the film is optimal when the bias voltage is −60 V. X-ray diffraction (XRD) analysis was performed on the samples with the optimal smoothness, and it was found that when the nitrogen flow rate was higher than 2 sccm, the titanium nitride film had a mixed phase of TiN(111) and (200). It is further revealed that the change of peak intensity of TiN(200) can be enhanced by nitrogen flow. Through atomic force microscopy (AFM), it is found that the stronger the intensity of the TiN (200) peak, the smoother the surface of the film is. Finally, the effect of different film thicknesses on the hardness and toughness of the TiN/Si3N4 film system was studied by nanoindentation experiments. The nanohardness (H) of the TiN/Si3N4 film can reach 39.2 GPa, the elastic modulus (E) is 480.4 GPa, the optimal toughness value (H3/E2) is 0.261 GPa, and the sample has good insulation performance. Linear fitting of the film’s toughness to nanohardness shows that TiN/Si3N4 films with higher hardness usually have a higher H3/E2 ratio.
With the application of a three-dimensional (3D) characterization technique, serial block-face scanning electron microscopy (SBFSEM), the 3D microstructure of a hydrated cement monomineral, tricalcium silicate (C3S), was measured with nanoscale resolution. The 3D morphologies of anhydrous particles, hydrated products, and capillary pores were visualized. Closed and open pores were discovered inside an anhydrous particle. The size and distribution of both the anhydrous C3S particles and their capillary pores were analyzed quantitatively and the porosity was determined to be 9%. The distribution of pores was found to be in a good agreement with the inner and outer product model of Hu et. al., with an inner shell distance of 860 nm. Considering the spatial resolution of the instrument and the volume of sample measured, most pores in this experiment could be characterized as capillary pores.
The in vivo fast degradation and poor biocompatibility are two major challenges of the magnesium alloys in the field of artificial bone materials. In this study, graphene oxide (GO) was first functionalized by chitosan (GOCS) and then immobilized on the magnesium alloy surface, finally the complex of heparin and bone morphogenetic protein 2 was incorporated on the modified surface to synergistically improve the corrosion resistance, anticoagulation, and osteogenesis. Apart from an excellent hydrophilicity after the surface modification, a sustained heparin and BMP2 release over 14 days was achieved. The corrosion resistance of the modified magnesium alloy was significantly better than that of the control according to the results of electrochemical tests. Moreover, the corrosion rate was also significantly reduced in contrast to the control. The modified magnesium alloy not only had excellent anticoagulation, but also can significantly promote osteoblast adhesion and proliferation, upregulate the expression of alkaline phosphatase and osteocalcin, and enhance mineralization. Therefore, the method of the present study can be used to simultaneously improve the corrosion resistance and biocompatibility of the magnesium alloys targeted for the orthopedic applications.
A serial block-face scanning electron microscopy (SBFSEM) system, composed of a scanning electron microscope (SEM) and an ultra-microtome installed within the SEM vacuum chamber, has been used to characterize the three-dimensional (3D) microstructure of tricalcium silicate (C3S) grains embedded in epoxy resin. A selection of C3S grains were segmented and rendered with 3D-image processing software, which allowed the C3S grains to be clearly visualized and enabled statistically quantitative analysis. The results show that about 5% of the C3S grains have volumes larger than 1 μm3 and the average volume of the grains is 25 μm3. Pores can also be clearly seen in the biggest C3S grain, the volume of which is 3.6 × 104 μm3, and the mean volume and total volume of all the pores within this grain are 4.8 μm3 and 3.0 × 103 μm3, respectively. The reported work provides a new approach for the characterization of the 3D spatial structure of raw C3S materials, and the resulting 3D structure of the raw C3S is important for further systematic research on the relationships between the spatial microstructure and the hydration kinetics of C3S and other cement minerals.
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