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Commercially pure titanium (cp Ti) is widely used in dental implantology. However, it is only passively integrated in bone and the resulting fixation in the bone, which is necessary for the function, is mainly mechanical in its nature. With the objective of increasing the chemical interaction between the implant and bone tissue, several phosphonic acids were synthesized and grafted onto titanium disks. The bare polished Ti disks (Ti P) and the grafting of three phosphonic acids (methylenediphosphonic acid (MDP), propane-1,1,3,3-tetraphosphonic acid (PTP), and ethane-1,1,2-triphosphonic acid (ETP)) on these disks were characterized with X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). These surface analytical techniques provided strong indications of the formation of a chemical link between the Ti implant and the phosphonic acid molecule. The bioactivity of the modified Ti disks was evaluated by incubating these disks in a physiological solution (Hank's balanced salt solution (HBSS)) for 1, 7, and 14 days. Modified surfaces showed only slightly higher calcium levels in the XPS analysis compared to the reference Ti P surface. Among them, the surface modified with ETP (Ti P + ETP) induced the highest calcium phosphate deposition after 14 days incubation.

Glow discharge plasma treatment is a frequently used method for cleaning, preparation, and modification of biomaterial and implant surfaces. The merits of such treatments are, however, strongly dependent on the process parameters. In the present work the possibilities, limitations, and risks of plasma treatment for surface preparation of metallic materials are investigated experimentally using titanium as a model system, and also discussed in more general terms. Samples were treated by different low-pressure direct current plasmas and analyzed using Auger electron spectroscopy (AES), x-ray photoelectron spectroscopy (XPS), atomic force microscopy, scanning electron microscopy, and light microscopy. The plasma system is a home-built, ultra-high vacuum-compatible system that allows sample introduction via a load-lock, and precise control of pressure, gas composition and flow rate, etc. This system allows uniform treatment of cylindrical and screw-shaped samples. With appropriate plasma parameters, argon plasma remove all chemical traces from former treatments (adsorbed contaminants and other impurities, and native oxide layers), in effect producing cleaner and more well-controlled surfaces than with conventional preparation methods. Removal (sputtering) rates up to 30 nm/min are possible. However, when inappropriate plasma parameters are used, the result may be increased contamination and formation of unintentional or undesired surface layers (e.g., carbides and nitrides). Plasma-cleaned surfaces provide a clean and reproducible starting condition for further plasma treatments to form well-controlled surface layers. Oxidation in pure O 2 (thermally or in oxygen plasmas) results in uniform and stoichiometric TiO 2 surface oxide layers of reproducible composition and thicknesses in the range 0.5-150 nm, as revealed by AES and XPS analyses. Titanium nitride layers were prepared by using N 2 plasmas. While mild plasma treatments leave the surface microstructure unaffected, heavy plasma treatment can give rise to dramatic morphologic changes.Comparison of these results with corresponding analyses of commercial implants and electropolished and/or anodically oxidized samples shows that the plasma treatment offers superior control of the surface status. However, it is also shown that improper control of the plasma process can produce unwanted and irreproducible results.

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A d.c. oxygen glow discharge was used to modify medical-grade poly(vinyl chloride) (PVC) to study how surface chemistry and hydrophilicity influence Pseudomonas aeruginosa adhesion. The effects of plasma exposure time on the resulting surface, including chemical composition, wettability and roughness, were assessed using x-ray photoelectron spectroscopy, contact angle measurements and atomic force microscopy analysis. A significant alteration in the hydrophilicity of the native PVC surface was observed after oxygen glow discharge treatment. The water contact angle decreased from ∼80• to 8-20• , with a weak dependence of the exposure time used. The change in surface wettability resulted from the incorporation of oxygenated functional groups, including esters, ketones and acids, as indicated by XPS analysis. The amount of oxygen incorporation was shown to be essentially independent of plasma exposure time. However, prolonged plasma exposure resulted in increased surface roughness. Bacterial adhesion efficiency was evaluated for PVC modified by 120 s of plasma exposure, because this exposure time was determined to yield the maximum decrease in contact angle. Oxygen plasma treatment of native PVC was found to yield a 70% reduction in bacterial adhesion for the four strains of Pseudomonas aeruginosa tested.

Diamond-like carbon (DLC) and silicon carbide (SiC) coatings are attractive because of low friction coefficient, high hardness, chemical inertness and smooth finish, which they provide to biomedical devices. Silicon wafers (Si waf ) and silicone rubber (Si rub ) plates were coated using plasmaenhanced chemical vapour deposition (PE-CVD) techniques. This article describes: 1-the characterization of modified surfaces using attenuated total reflection-Fourier transform infrared spectroscopy (ATR/FTIR) and contact angle measurements, 2-the results of three in-vitro haemocompatibility assays. Coated surfaces were compared to uncoated materials and various substrates such as polymethylmethacrylate (PMMA), polyethylene (LDPE), polydimethylsiloxane (PDMS) and medical steel (MS). Thrombin generation, blood platelet adhesion and complement convertase activity tests revealed the following classification, from the most to the least heamocompatible surface: Si rub / DLC-Si rub / DLC-Si waf / LDPE/ PDMS/ SiCSi waf / Si waf / PMMA/ MS. The DLC coating surfaces delayed the clotting time, tended to inhibit the platelet and complement convertase activation, whereas SiC-coated silicon wafer can be considered as thrombogenic. This study has taken into account three events of the blood activation: coagulation, platelet activation and inflammation. The response to those events is an indicator of the in vitro haemocompatibility of the different surfaces and it allows us to select biomaterials for further in vivo blood contacting investigations.

Titanium is widely used in dental implants due to its suitable physical properties and its good biocompatibility. However, it is integrated into bone only passively, and the resulting fixation in the bone, which is necessary for the function, is mainly mechanical in nature. With the objective of increasing the chemical interaction between the implant and the bone tissue, several phosphonic acids were synthesized and grafted onto titanium disks. Here we report on the proliferation, differentiation, and protein production of rat osteoblastic cells (CRP10/30) on phosphonic-acid-modified titanium surfaces studied in vitro. No statistical differences were found in osteoblast proliferation among the phosphonic-acid-modified titanium, unmodified titanium, and tissue culture plastic (used as a positive control), indicating that the phosphonic acids used were not cytotoxic to the osteoblasts used. For all surfaces (modified or not), the alkaline phosphatase activity was at least as good as it was on tissue culture plastic. However, the total amount of protein, and especially the collagen type I synthesis, was sensitive to surface modification. On titanium modified with ethane-1,1,2-triphosphonic acid, the total amount of synthesized protein was significantly higher than it was on unmodified titanium surfaces. A significant increase (up to 16%) of collagen type I production was observed on titanium surfaces modified with this acid or with methylenediphosphonic acid compared to unmodified titanium surfaces.

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