Calcium silicate-based sealers were recently introduced as a new class of endodontic sealers, with potential further benefits due to their bioactivity. The aim of this study was to evaluate the biocompatibility of two new hydraulic calcium silicate-based sealers, TotalFill BC Sealer (FKG, La Chaux-des-Fonds, Switzerland) and TotalFill BC Sealer HiFlow (FKG, La Chaux-des-Fonds, Switzerland) through subcutaneous implantation in connective tissue of rats. Subcutaneous implantation was performed in 16 young Wistar rats. Four polyethylene tubes were implanted in each animal, one empty to serve as a control, and three filled with tested sealers: AH Plus as reference (Dentsply DeTrey, Konstanz, Germany), TotalFill BC Sealer (BC) and TotalFill BC Sealer HiFlow (HiFlow). Eight rats were euthanized at 8 days and the remaining eight at 30 days. Hematoxylin-eosin staining was used to score the inflammatory reaction, macrophage infiltrate and to measure the thickness of the fibrous capsule. von Kossa staining was performed to evaluate the mineralization level. Kruskal–Wallis test followed by Dunn’s post hoc test was used to analyze non-parametric data. To analyze the influence of the implantation time within each material, a Mann–Whitney U test was performed. At eight days post-implantation, AH Plus induced a more intense inflammatory reaction when compared both with the control (p $\le$ 0.001) and BC (p $\le$ 0.01). HiFlow presented a higher score of macrophage infiltrate than control (p $\le$ 0.01) and BC (p $\le$ 0.05). The fibrous capsule thickness in this period was significantly higher for the BC group when compared to control (p $\le$ 0.01) and AH Plus (p $\le$ 0.05). The mineralization potential was higher for the HiFlow group when compared with the control (p $\le$ 0.001) and AH Plus (p $\le$ 0.001). At 30 days post-implantation, the score for the inflammatory reaction remained higher for the AH Plus group when compared both to control (p $\le$ 0.01) and BC (p $\le$ 0.001). The macrophage infiltrate of the HiFlow was significantly higher than control (p $\le$ 0.001) and AH Plus groups (p $\le$ 0.01), additionally, the fibrous capsule of the BC (p $\le$ 0.001) and HiFlow (p $\le$ 0.01) groups were both thicker than control. Mineralization potential was observed only on BC (p $\le$ 0.05) and HiFlow groups (p $\le$ 0.001), when compared to control). BC exhibited the best biocompatibility performance of all tested sealers and HiFlow provided the greatest induction of mineralized tissues. Both TotalFill BC Sealer and TotalFill BC Sealer HiFlow are biocompatible and show potential bioactivity when implanted in the subcutaneous tissue. Bioactivity was not found in AH Plus.

The orthodontic supply market is a prosperous billion-dollar industry, driven by an increasing demand for orthodontic appliances. The supremacy of metallic first-generation biomaterials is evident for manufacturing brackets, archwires, bands, and other components due to their well-recognized chemical inertness, spontaneous passivation, biocompatibility, and favorable mechanical properties combination. However, the oral cavity is the ultimate corrosion-promoting environment for any metallic material. In this work, the general picture of the intraoral degradation of fixed orthodontic appliances is first addressed, from the causes to the harmful effects and their oral clinical implications. Current mitigation strategies are also pointed out, including the alloys’ bulk composition adjustment combined with new and advanced manufacturing processes and/or their surface treatment or coating deposition. The versatile use of thin films and coatings stands out with different deposition technologies: Many in vivo and in vitro efforts have been devoted to oral aging, from monolithic to composite architectures and micro- to nano-scale materials, to meet the best and safest oral practice demands. Unfortunately, literature data suggest that even the existing commercially available protective coatings have drawbacks and are fallible. Further multidisciplinary research is still required to effectively mitigate the corrosion behavior of fixed orthodontic appliances.

Stainless steels (SS) are the most-used alloys for manufacturing fixed orthodontic appliances due to their attractive set of mechanical properties, biocompatibility, and high corrosion resistance. Nevertheless, during regular orthodontic treatments–taking at least around 2 years–the intraoral environment inevitably degrades these bioalloys, releasing metallic ions into the oral cavity. In the first part of this in vitro study, the corrosion resistance of commercial SS appliances (brackets, tubes, and bands) was evaluated in Fusayama-Meyer artificial saliva at pH values of 2.3 and 6.8 over the course of 30 days. As expected, the results corroborated that salivary pH highly influences corrosion behaviour. Released Ni, Cr, and Fe were within dietary intake values. In the second part, a novel approach for oral corrosion prevention based on the chemical inertness of DLC materials is presented. SS surfaces were functionalized with biocompatible a-C:H-sputtered coatings and submitted to the same experimental conditions. The anticorrosion ability of this system was demonstrated, preventing the pitting corrosion that occurred on the SS substrates. Despite the galvanic coupling effect due to the presence of the Cr-based interlayer, this study enhanced the potential use of the reactive sputter-deposited a-C:H coatings in orthodontics.

Hydrogenated amorphous carbon (a-C:H) coatings are attractive materials for protecting metallic surfaces in extreme biological environments like the human oral cavity, due to the unusual combination of mechanical properties, superior bioinertness, and relative easier and cheaper production. In this work, two a-C:H coatings were deposited on AISI 316L substrates by reactive magnetron sputtering with two CH₄ flows to assess if this outstanding system could extend its application range to orthodontics. A 30-day immersion test in Fusayama-Meyer artificial saliva was conducted to mimic an extreme acidic intraoral pH. Extracts were quantified and used to perform in vitro assays with mono- and co-cultures of macrophages and fibroblast to assess cell viability, while mechanical and structural behaviors were studied by nanoindentation and visible Raman. The empirically estimated H contents of ~28 and 40 at.% matched the hard and soft a-C:H coating regimes of 18 and 7 GPa, respectively. After immersion, no important structural/mechanical modifications occurred, regardless of the H content, without corrosion signs, delamination, or coating detachment. However, the adhesion-promoting Cr-based interlayer seems to reduce corrosion resistance via galvanic coupling. The highest biocompatibility was found for a-C:H coatings with the lowest H content. This study indicates that sputtered a-C:H are promising surface materials in orthodontics.

Hydrogenated amorphous carbon (a-C:H) has been considered a promising biocompatible coating to protect metallic alloys against corrosion for medical applications, namely orthodontics. However, there is still no optimal solution for this biomedical field; hence, the investigation remains open. In this work, the effect of a nonmetallic doping element (N) on sputter-deposited a-C:H coatings was studied concerning both salivary corrosion and cytotoxicity behavior. After a 30-day corrosion test in an acidic modified Fusayama-Meyer artificial saliva, metal release from both coated and uncoated 316L stainless steel (SS) substrates was quantified. Tests on the corrosion extracts were then performed by using monocultures of macrophages and fibroblasts, and their coculture; and cell viability was evaluated via the MTT test. Results show an overall inhibition of the SS corrosion, which enhanced the in vitro biocompatibility with a minimal effect on the coatings’ microstructure. Among all the coatings tested, the undoped a-C:H coating performed the best, whereas an increase in N doping led to poorer protection against metal dissolution and a subsequent slightly lower biocompatibility. The findings corroborate that selecting the nonmetallic element N for doping C-based coatings is not a good choice for this biomedical field, even at low contents up to 10 at.%.