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Ti Nano-nodular Structuring for Bone Integration and Regeneration

¹ Laboratory for Bone and Implant Sciences (LBIS), The Jane and Jerry Weintraub Center for Reconstructive Biotechnology, Division of Advanced Prosthodontics, Biomaterials and Hospital Dentistry, UCLA School of Dentistry, 10833 Le Conte Avenue (B3-081 CHS), Box 951668, Los Angeles, CA 90095-1668, USA; and
² Department of Oral Anatomy, Aichi-Gakuin University, School of Dentistry, Nagoya, Japan

View larger version (108K): [in this window] [in a new window]   Figure 1. Nano-nodular self-assembly of titanium on variously pre-micro-roughened titanium surfaces. (A) Scanning electron microscopic (SEM) x10,000 images before and after electron-beam physical vapor deposition (EB-PVD) of titanium for 16 min 40 sec, with a deposition rate of 5 Å / sec onto various titanium surfaces. Images in gray indicate no or little nano-nodules created, while images highlighted in blue indicate dense, uniform, and consistent nano-nodules. Titanium substrates (disks of 20 mm in diameter) were prepared by the following: machining (Machined), hydrofluoric-acid-etching (HF), sand-blasting, hydrofluoric acid and sulfuric acid dual-etching (HF-H2SO4), sulfuric-acid-etching (H2SO4), and hydrochloric acid and sulfuric acid dual-etching (HCl-H2SO4). Bar = 2 µm and applies to all panels. (B) Atomic force micrographs of the various Ti substrates tested, showing various degrees of micro-roughness before titanium deposition (top images). The images are presented in a fixed vertical scale of 1.5 µm. Nano-structuring was unsuccessful in the first two substrates (A). Histograms show the results of quantitative roughness analysis for the substrates before Ti deposition: root mean-square roughness; peak-to-valley roughness; inter-irregularity space. Data are shown as mean ± standard deviation (n = 5). The blue bars indicate the substrates that resulted in nano-nodular creation, while the gray bars indicate the substrates that created few or no nano-nodules.

View larger version (99K): [in this window] [in a new window]   Figure 2. Size and height control of nano-nodular structure by adjustment of the deposition time and expanded surface areas by the nano-nodules. (A) Scanning electron microscopic images after Ti electron-beam physical vapor deposition (EB-PVD) onto the acid-etched titanium for various deposition times, showing the sizes of nano-nodules correlated with the deposition times. The nano-nodule outbreaks occurred in a time period as short as 3 min 20 sec. The deposition rate was fixed at 5 Å /sec. Images are at x10,000 magnification. Bar = 2 µm (all panels). (B) Atomic force micrographs of the Ti nano-structures created in panel A. (C) Nano-nodular structure AFM profiling. The diameter (arrow) and peak-to-valley distance (arrowhead) of the nano-nodules were measured manually, by side-by-side analysis of two-dimensional images and profiles of the titanium surfaces. The diameter (D) and peak-to-valley distance (E) of nano-nodules generated by different deposition times. Data are shown as mean ± standard deviation (n = 9). (F) Three-dimensional surface area of the nano-nodular surfaces measured in the field of 5 mm x 5 mm. Four different nano-surfaces created by different deposition times. Data are shown as mean ± standard deviation (n = 9).

View larger version (84K): [in this window] [in a new window]   Figure 3. Titanium nano-nodular assembly on non-metallic surfaces: polymer, glass, and biomaterials. Scanning electron micrographs showing the original non-metallic substrates and successful Ti nano-nodules created on the substrates (blue panels). Ti was deposited for 16 min 40 sec onto the original or sand-blasted surfaces of polystyrene, glass, collagen membrane, and poly-lactic acid (PLA), by electron-beam physical vapor deposition (EB-PVD). Images in gray represent unsuccessful nano-nodule assembly. Images are at x10,000 magnification. Bar = 2 µm (all panels).

View larger version (11K): [in this window] [in a new window]   Figure 4. Nano-nodular-enhanced bone-titanium integration evaluated by a biomechanical push-in test. Push-in values of the acid-etched and nano-nodular-structured implants at week 2 of healing are shown as the mean ± SD (n = 5). The diameter of the nano-nodules created for this in vivo testing was 560 nm. Statistically significant at *p < 0.001.