Two bovine hydroxyapatites (BHAs), one with granule size of 150 to 200 microm and one with granule size of 300 to 329 micro, and 2 synthetic hydroxyapatites (SHAs), with granule size of 150 and 300 microm, respectively, were compared for effectiveness in repairing circumferential bone defects in dogs. The hydroxyapatites (HAs) were characterized through powder x-ray diffraction (XRD) analysis and scanning electron microscopy (SEM). Three trephined bone defects (5.0 mm wide x 4 mm long) were created in the humeruses of 8 dogs. In a random manner, the defects on each side were treated with either BHA with small granules (BHA[s]), BHA with large granules (BHA[L]), SHA with small granules (SHA[s]), SHA with large granules (SHA[L]), or left to heal unaided (bilateral control). Four dogs were sacrificed after 6 and 12 postoperative weeks, respectively. Ground sections of each defect were submitted to histologic and histomorphometric analysis (percentage of area occupied by bone, bone marrow, and biomaterial). As a rule, the HA granules exhibited direct bone contact, regardless of the origin and the size of the granules. Control sites were related and had an increased amount of connective tissue infiltration. At 12 weeks, BHA(s) exhibited improved bone formation compared with SHA(s) and SHA(L). The SHA(s) delivered reduced amounts of bone compared with the remaining groups (control included). The area of bone measured in BHA(s) sites was significantly higher at 12 weeks than 6 weeks. The XRD revealed the tested HA samples to be highly crystalline, while BHA appeared with rougher surface at SEM analysis. The BHA(s) performed better than the SHA(s) and SHA(L), as assessed by the amount of bone measured in both implantation sites at 12 weeks. The BHA's material characteristic itself rather than granules size accounted for the distinctive biological behavior. The increased roughness of the BHAs' surface, as assessed through SEM, seemed to benefit the osteoconduction process.
Chitosan, which is a non-toxic, biodegradable and biocompatible biopolymer, has been widely researched for several applications in the field of biomaterials. Calcium phosphate ceramics stand out among the so-called bioceramics for their absence of local or systemic toxicity, their non-response to foreign bodies or inflammations, and their apparent ability to bond to the host tissue. Hydroxyapatite (HA) is one of the most important bioceramics because it is the main component of the mineral phase of bone. The aim of this work was to produce chitosan membranes coated with hydroxyapatite using the modified biomimetic method. Membranes were synthesized from a solution containing 2% of chitosan in acetic acid (weight/volume) via the solvent evaporation method. Specimens were immersed in a sodium silicate solution and then in a 1.5 SBF (simulated body fluid) solution. The crystallinity of the HA formed over the membranes was correlated to the use of the nucleation agent (the sodium silicate solution itself). Coated membranes were characterized by means of scanning electron microscopy-SEM, X-ray diffraction-XRD, and Fourier transform infrared spectroscopy-FTIR. The results indicate a homogeneous coating covering the entire surface of the membrane and the production of a semi-crystalline hydroxyapatite layer similar to the mineral phase of human bone.
Apatite coating was applied on titanium surfaces modified by Nd:YVO 4 laser ablations with different energy densities (fluency) at ambient pressure and atmosphere. The apatites were deposited by biomimetic method using a simulated body fluid solution that simulates the salt concentration of bodily fluids. The titanium surfaces submitted to the fast melting and solidification processes (ablation) were immersed in the simulated body fluid solution for four days. The samples were divided into two groups, one underwent heat treatment at 600 • C and the other dried at 37 • C. For the samples treated thermally the diffractograms showed the formation of a phase mixture, with the presence of the hydroxyapatite, tricalcium phosphate, calcium deficient hydroxyapatite, carbonated hydroxyapatite and octacalcium phosphate phases. For the samples dried only the formation of the octacalcium phosphate and hydroxyapatite phases was verified. The infrared spectra show bands relative to chemical bonds confirmed by the diffraction analyses. The coating of both the samples with and without heat treatment present dense morphology and made up of a clustering of spherical particles ranging from 5 to 20 m. Based on the results we infer that the modification of implant surfaces employing laser ablations leads to the formation of oxides that help the formation of hydroxyapatite without the need of a heat treatment.
RESUMONeste trabalho investigou-se a modificação de superfície do titânio pela irradiação com feixe de Laser Nd:YAG. Os parâmetros do laser como a potência, o comprimento de onda, a frequência, a velocidade de varredura e a área de exposição foram mantidos constantes, exceto o espaçamento da matriz, o qual foi de 0,01 e 0,02 mm. A caracterização da superfície foi realizada por Microscopia Eletrônica de Varredura (MEV) e Difração de Raios X (DRX), sendo que os espectros foram refinados pelo método Rietveld. Pela análise de MEV, observou-se uma mudança na topografia, obtendo uma superfície rugosa produzida pelo fenômeno de ablação. As análises por Rietveld dos espectros de difração de raios X detectaram TiN, Ti 2 N, TiO 2 (anatásio e rutilo), sendo que a amostra com espaçamento 0,01 mm apresentou uma maior quantidade de óxidos e nitretos. Isso pode ser devido à sobreposição do feixe, induzindo à formação de uma superfície com maior estabilidade termodinâmica. Os óxidos e nitretos obtidos são de grande importância, pois são responsáveis por produzir uma maior interação entre o osso-implante.Palavras chaves: Laser Nd:YAG, titânio c.p., modificação de superfície, biomateriais. Influence of the Nd:YAG laser beam spacing in obtaining oxides and nitrides on titanium surface at atmospheric pressure ABSTRACTIn this work the titanium surface modification by Laser Nd:YAG irradiation was investigated. Laser parameters such as power, wavelength, frequency, scanning speed and the exposure area were maintained constant, except the matrix spacing, which was equal 0,01 and 0,02 mm. Characterization was carried out by Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) analysis, for which the spectra were refined by the Rietveld method. In the analysis by SEM, a change in the topography was observed, with a rough surface obtained by ablation phenomenon. The Rietveld analysis of the spectra presented the phases TiN, Ti2N, TiO2 (anatase and rutile), and the sample with spacing equal to 0,01 mm presented a larger amount of oxides and nitrides. This may be due to the beam overlapping, which induces a surface with larger thermodynamic stability. The oxides and nitrides are of great importance, because they are responsible for producing a satisfactory interaction between the bone and the implant.
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