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(1) Background: The desire to avoid autograft harvesting in implant dentistry has prompted an ever-increasing quest for bioceramic bone substitutes, which stimulate osteogenesis while resorbing in a timely fashion. Consequently, a highly bioactive silicon containing calcium alkali orthophosphate (Si-CAP) material was created, which previously was shown to induce greater bone cell maturation and bone neo-formation than β-tricalcium phosphate (β-TCP) in vivo as well as in vitro. Our study tested the hypothesis that the enhanced effect on bone cell function in vitro and in sheep in vivo would lead to more copious bone neoformation in patients following sinus floor augmentation (SFA) employing Si-CAP when compared to β-TCP. (2) Methods: The effects of Si-CAP on osteogenesis and Si-CAP resorbability were evaluated in biopsies harvested from 38 patients six months after SFA in comparison to β-TCP employing undecalcified histology, histomorphometry, and immunohistochemical analysis of osteogenic marker expression. (3) Results: Si-CAP as well as β-TCP supported matrix mineralization and bone formation. Apically furthest away from the original bone tissue, Si-CAP induced significantly higher bone formation, bone-bonding (bone-bioceramic contact), and granule resorption than β-TCP. This was in conjunction with a higher expression of osteogenic markers. (4) Conclusions: Si-CAP induced higher and more advanced bone formation and resorbability than β-TCP, while β-TCP’s remarkable osteoconductivity has been widely demonstrated. Hence, Si-CAP constitutes a well-suited bioactive graft choice for SFA in the clinical arena.
The surface of a titanium alloy (Ti6Al4V) implant material was covered with a bioactive calcium alkali phosphate ceramic with the aim to accelerate the healing and to form a stronger bond to living bone tissue. To fix the ceramic powder we used a femtosecond laser, which causes a thin surface melting of the metal. It is a requirement to prove that the laser irradiation would not reduce the lifetime of implants. Here we present the results of mechanical stability tests, determined by the rotating bending fatigue strength of sample rods. After describing the sample surfaces and their modifications caused by the laser treatment we give evidence for an unchanged mechanical stability. This applies not only to the ceramic fixation but also to a comparatively strong laser ablation.
Calcium alkaline phosphate scaffolds for bone regeneration 3D-fabricated by additive manufacturing
(2012)
Calcium alkaline phosphate granulates can be used for substitution of several bone defects but for the reconstruction of large skeletal parts in the maxillofacial and orthopaedic fields fitted scaffolds are preferable. Within the additive manufacturing methods, the 3D printing process offers exciting opportunities to generate defined porous scaffolds. We used a R1 printer from ProMetal Company, USA, for producing scaffolds directly from a ceramic powder. For this direct free form fabrication technology the powder has to possess a lot of specific properties both for the generation of a stable green body and also for the subsequent sintering preparation. For this printing process we prepared different granules in a fluidized bed process containing Ca2KNa(PO4)2 as main crystalline phase. Granules were characterized by different methods and several sieve fractions were used for preparing disc like and cylindrical parts. The suitability of granules for this printing process was determined by porosity and strength of produced bodies. Next to granules' performance both of these properties can be directly influenced by 3D printing process parameters. With knowledge of suitable process parameters scaffolds with different porosity in a respective desired design can be created. In this study, cylindrical scaffolds with graded porosity were produced for bone regeneration of segmental defects in maxillofacial surgery and dental implantology by tissue engineering.
Several substituted β-tricalcium phosphates have been prepared with different cations (monovalent, divalent and trivalent) and at various levels of substitution. Structural investigations have proved that fewer than ~10% wt substitution, the substituted compounds are isostructural to β-TCP, leading to solid solutions. These samples have been characterized by infrared and Raman spectroscopies. The vibrational spectra show mainly the bands related to the vibrations of PO43- tetrahedrons present in the structure. As Raman scattering and infrared absorption are local probes, the bands are sensitive to the local environment of the distinct tetrahedrons, related to the site of substitution and to the nature of the cations.
Calcium alkaline phosphate scaffolds for bone regeneration 3D-fabricated by additive manufacturing
(2011)
In this paper, we report X-ray diffraction investigations as well as Raman and solid-state 31P and 23Na magic angle spinning nuclear magnetic resonance (NMR) characterization of three series of calcium orthophosphates. The general formulae of the studied compounds are Ca10.5-x/2Mx(PO4)7, where M = K or Na and x = 0, 0.25, 0.50, 0.75, 1.0; and Ca10KxNa1-x(PO4)7, where x = 0, 0.25, 0.5, 0.75, 1.0. These calcium orthophosphates are found to be isostructural with β-tricalcium phosphate (β-TCP, Ca3(PO4)2) with the substitution of some calcium sites by potassium and/or sodium cations. The unit cell parameters vary continuously with the level of substitution, a characteristic of these solid solutions. The Raman spectra show the different vibrational bands of the phosphate groups PO4, while the NMR chemical shifts are sensitive to the non-equivalent phosphorus and sodium ions present in these substituted samples. As both Raman and NMR spectroscopies are local probes, they offer tools to distinguish between these different phosphorus and phosphate groups, according to their structural site and local environment, especially the type of cation substituent. A convenient decomposition of the Raman and NMR spectra into GaussianLorentzian components leads us to propose an assignment of the main observed bands of these substituted β-TCPs.
Bone implants made of metal, often titanium or the titanium alloy Ti6Al4V, need to be surface treated to become bioactive. This enables the formation of a firm and durable connection of the prosthesis with the living bone. We present a new method to uniformly cover Ti6Al4V with a thin layer of ceramics that imitates bone material. These calcium alkali phosphates, called GB14 and Ca10, are applied to the metal by dip coating of metal plates into an aqueous slurry containing the fine ceramic powder. The dried samples are illuminated with the 790 nm radiation of a pulsed femtosecond laser. If the laser fluence is set to a value just below the ablation threshold of the ceramic (ca. 0.4 J/cm²) the 30 fs laser pulses penetrate the partly transparent ceramic layer of 20–40 µm thickness. The remaining laser fluence at the ceramic–metal interface is still high enough to generate a thin metal melt layer leading to the ceramic fixation on the metal. The laser processing step is only possible because Ti6Al4V has a lower ablation threshold (between 0.1 and 0.15 J/cm²) than the ceramic material. After laser treatment in a fluence range between 0.1 and 0.4 J/cm², only the particles in contact with the metal withstand a post-laser treatment (ultrasonic cleaning). The non-irradiated rest of the layer is washed off. In this work, we present results of a successful ceramic fixation extending over larger areas. This is fundamental for future applications of arbitrarily shaped implants.
Porous ceramics prepared by the foam replication technique have a high porosity and low mechanical stability. It has been reported that coating such porous ceramics with gelatin allows for an improved compressive strength. Little details regarding the influence of important gelatin parameters such as concentration, temperature and drying conditions as well as bloom number which is a measure of the gel rigidity, on this toughening effect are available. This paper investigates the influence of these parameters on compressive strength of gelatin coated porous hydroxyapatite ceramics. It was found that concentration in the gelatin sols has a marked impact whereas sol temperature, bloom number and differing conditions during subsequent drying have only little influence on the compressive strength of the coated ceramics.