Bioactive composites containing TEGDMA-functionalized calcium phosphate particles: Degree of conversion, fracture strength and ion release evaluation.

OBJECTIVE: To evaluate the strength and ion release of experimental composites containing TEGDMA-functionalized calcium phosphate particles. METHODS: Seven composites containing equal parts (in mols) of BisGMA and TEGDMA and 60vol% of fillers were manipulated. Filler phase was constituted by silanized barium glass and 0% (control), 10% or 20% (volume) of dicalcium phosphate dihydrate (DPCD) particles, either non-functionalized or functionalized with two different TEDGMA contents. DCPD particles were synthesized and characterized by X-ray diffraction (XRD), elemental analysis, surface area and dynamic light scattering. Composites were tested for degree of conversion (DC) by near-FTIR. Biaxial flexural strength (BFS) was determined after 24h and 28days in water. Calcium and phosphate release after 7days was assessed using inductively coupled plasma optical emission spectrometry (ICP-OES). Data were analyzed by ANOVA/Tukey test (alpha:5%). RESULTS: XRD confirmed the crystalline structure corresponding to DCPD. Elemental analysis revealed particles with zero, 14% or 22% TEGDMA, with similar D50 (around 19µm) and surface areas from 3.5 to 11.4m2/g. The presence of DCPD did not reduce DC. After 24h, functionalization (both 14% and 22% TEGDMA) improved composite strength in comparison to non-functionalized DCPD, both at 10% and 20% levels. After 28days, BFS of materials containing 10% functionalized DCPD were statistically similar to the control containing only barium glass. Among composites containing 10% DCPD, particle functionalization with 14% TEGDMA did not jeopardize ion release. SIGNIFICANCE: At 10vol%, the use of TEGDMA-functionalized CaP particles improved composite strength in relation to non-functionalized particles, while maintaining similar ion release levels.

Physico-chemical characterization of zirconia-titania composites coated with an apatite layer for dental implants.

OBJECTIVES: To investigate the crystalline phases, morphological features and functional groups on the surface of sintered Y:TZP/TiO2 composite ceramics before and after the application of a biomimetic bone-like apatite layer. The effect of TiO2 content on the composite's characteristics was also evaluated. METHODS: Samples of Y:TZP containing 0-30mol% TiO2 were synthesized by co-precipitation, followed by filtration, drying and calcination. The powders were uniaxially pressed and sintered at 1500°C/1h. To obtain biomimetic coatings the samples were exposed to sodium silicate solution and then to a concentrated simulated body fluid solution. The surfaces, before and after coating, were characterized by diffuse reflectance infrared Fourier transformed spectroscopy, X-ray diffraction analysis and scanning electron microscopy. RESULTS: The surfaces of all Y:TZP/TiO2 samples were covered with a dense and uniform calcium phosphate layer with a globular microstructure. This layer was crystalline for specimens with 30% of TiO2 and amorphous for specimens with 0 and 10% of TiO2. Chemical analysis indicated that this layer was composed of type A carbonate apatite. Among the materials tested, the composite with 10% of TiO2 showed the best overall chemical and physical features, such as higher density and more cohesive amorphous apatite layer. SIGNIFICANCE: Y-TZP-based materials obtained in the present investigation by means of the successful association of a calcium phosphate biomimetic layer with small amounts TiO2 should be further explored as an option for ceramic dental implants with improved bioactivity.

In vitro apatite formation on chemically treated (P/M) Ti-13Nb-13Zr.

OBJECTIVES: Titanium alloys are considered the material of choice when used as endosteal part of implants. However, they are not able to bond directly to bone. The objective of this study was to suggest a chemical surface treatment for Ti-13Nb-13Zr to initiate the formation of hydroxy carbonated apatite (HCA) during in vitro bioactivity tests in simulated body fluid (SBF). METHODS: Titanium, niobium, and zirconium hydride powders were blended, compacted and sintered. Sintered Ti-13Nb-13Zr samples were etched in HCl, H(3)PO(4), and in a mixture of HF+HNO(3), respectively, and subsequently pretreated in NaOH. The influence of acid etching conditions on the microstructure of the Ti-13Nb-13Zr alloys as well as on the rate of HCA formation was evaluated using SEM-EDS, FTIR, and gravimetric analyses. RESULTS: Sintered Ti-13Nb-13Zr alloys consist of a Widmannstätten (alpha+beta) microstructure. Exposure of chemically etched and NaOH activated samples to SBF for 1 week leads to the formation of a HCA layer on the surface of HCl as well as H(3)PO(4) treated samples. No HCA formation was found on HNO(3) treated samples. After 2 weeks in SBF the mass increase, that can be correlated to the HCA formation rate, was the highest for HCl pretreated samples (2.4 mg/cm(2)) followed by H(3)PO(4) (0.8 mg/cm(2)) and HNO(3) pretreated ones (0.2 mg/cm(2)). SIGNIFICANCE: Since the in vitro HCA formation from SBF is generally accepted as a typical feature for bioactive materials, it is supposed that HCl etching with subsequent NaOH treatment might enhance the in vivo bone-bonding ability of Ti-13Nb-13Zr.