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EN
Laser surface modification of titanium alloys is one of the main methods of improving the properties of titanium alloys used in implantology. This study investigates the microstructural morphology of a laser-modified surface layer on a Ti13Nb13Zr alloy with and without a carbon nanotube coating deposited by electrophoretic deposition. Laser modification was performed for samples with and without carbon nanotube coating for two different laser powers of 800 W and 900 W and for different scan rates: 3 mm/s or 6 mm/s at 25 Hz, and the pulse duration was 2.25 ms or 3.25 ms. A scanning electron microscope SEM was used to evaluate the surface structure of the modified samples. To observe the heat-affected zones of the individual samples, metallographic samples were taken and observed under an optical microscope. Surface wettability tests were performed using a goniometer. A surface roughness test using a profilograph and a nanoindentation test by NanoTest™ Vantage was also performed. Observations of the microstructure allowed to state that for higher laser powers the surfaces of the samples are more homogeneous without defects, while for lower laser powers the path of the laser beam is clearer and more regular. Examination of the microstructure of the cross-sections indicated that the samples on which the carbon nanotube coating was deposited are characterized by a wider heat affected zone, and for the samples modified at 800 W and a feed rate of 3 mm/s the widest heat affected zone is observed. The wettability tests revealed that all the samples exhibit hydrophilic surfaces and the samples with deposited carbon nanotube coating increase it further. Surface roughness testing showed a significant increase in Ra for the laser-modified samples, and the presence of carbon nanotubes further increased this value. Nanoindentation studies showed that the laser modification and the presence of carbon coating improved the mechanical properties of the samples due to their strength.
2
Content available remote The influence of laser alloying of Ti13Nb13Zr on surface topography and properties
EN
The laser alloying is a continually developing surface treatment because of its significant and specific structuration of a surface. In particular, it is applied for Ti alloys, being now the most essential biomaterials` group for load-bearing implants. The present research was performed on the Ti13Nb13Zr alloy subject to laser modification in order to determine the treatment effects on surface topography and its some mechanical properties like nanohardness, Young's modulus, roughness. A pulse laser Nd:YAG was applied at three different laser pulse regimes: either 700 W, 1000 W or 1000 W treatment followed by 700 W modification at a pulse duration of 1 ms. The surface topography and morphology were examined using light microscopy and scanning electron microscopy with spectroscope of X-ray energy dispersion. The mechanical properties were determined by nanoindentation tests and surface roughness with a use of profilograph. The wettability was tested with a goniometer. The obtained results demonstrate complex behavior of the material surface: decrease in penetration distance and increase in hardness after first laser treatment, maintenance of this trend when machining using a higher laser pulse power, followed by an increase in penetration and decrease in hardness after additional laser treatment at lower power input, due to which a surface with fewer defects is obtained. The change in Young`s modulus follows the change in other mechanical properties, but not a change in roughness. Therefore, the observed hardening with the increase of the laser pulse power and then a small softening with the use of additional treatment with lower power can be attributed to some processes of remelting, diffusion and crystallization, sensitive to the previous surface state and heat energy flux. Despite that, the laser treatment always caused a significant hardening of the surface layer.
PL
Do eksperymentu użyto stopu tytanu Ti13Nb13Zr, który ze względu na swój skład chemiczny i właściwości mechaniczne stanowi materiał do zastosowań w inżynierii medycznej. Celem pracy była ocena wpływu stopowania laserowego stopu Ti13Nb13Zr z powłoką z wielościennych nanorurek węglowych na jego właściwości mechaniczne (chropowatość, nanotwardość, moduł Younga). Do wytworzenia powłoki węglowej wykorzystano metodę osadzania elektroforetycznego (EDP). Modyfikację laserową przeprowadzono przy użyciu impulsowego lasera Nd:YAG. Zastosowano moc impulsu 800 W i czas impulsu 0,5 ms oraz 1 ms. Właściwości mechaniczne zmierzono za pomocą nanoindentera, zaś chropowatość z użyciem mikroskopu sił atomowych (AFM). Zastosowanie powłoki z wielościennych nanorurek węglowych do stopowania laserowego stopu Ti13Nb13Zr oraz odpowiedni dobór parametrów procesu pozwoliły na podwyższenie właściwości mechanicznych (nanotwardość wzrosła ponad dwukrotnie) w stosunku do własności materiału rodzimego, nastąpiło również ujednolicenie właściwości w obrębie badanej powierzchni.
EN
The titanium alloy Ti13Nb13Zr was used as a substrate, because of its chemical composition and good mechanical properties in application of tissue engineering. The aim of the wark was the assessment of the influence of laser alloying of Ti13Nb13Zr coated with multi-walled carbon nanotubes for mechanical properties (roughness, nanohardness, Young modulus). Electrophoretic deposition (EOP) method was used to prepare carbon coating. Laser modification was carried out with Nd:YAG laser in pulsed mode operating system. The power of the impulse was 800 Wand the time 0,5 ms and 1 ms. Mechanical properties were checked with nanoindenter and roughness of the surface with Atomic Force Microscope (AFM). The improvement of mechanical properties (the nanohardness increases more than twice) and its homogeneity within tested area (in the comparisan to the native material) was seen after implementation of carbon nanotube coating with appropriate parameters of the process.
EN
The surface condition of an implant has a significant impact on response occurring at the implant-biosystem border. The knowledge of physical-chemical and biological processes allows for targeted modification of biomaterials to induce a specified response of a tissue. The present research was aimed at development of technology composing of obtaining the nanotube oxide layers on a porous titanium alloy Ti13Nb13Zr, followed by the deposition of phosphate coating. The porous substrate (porosity about 50%) was prepared by a selective laser melting of the Ti13Nb13Zr powder with the SLM Realizer 100 equipment. The nanotubular oxide layers were fabricated by electrochemical oxidation in H3PO4 + 0.3% HF mixture for 30 min. at a constant voltage of 20V. The calcium phosphate coatings were formed by the electrochemically assisted deposition (ECAD). The presence of nanotubular oxide layers with their internal diameters ranging from 30 to 100 nm was observed by SEM (JEOL JSM-7600F). The nanotubes have dimensions that facilitated the deposition of hydroxyapatite.
5
Content available remote Hydroxyapatite deposition on the laser modified Ti13Nb13Zr alloy
EN
The Ti13Nb13Zr alloy was subjected to laser modification with the Nd:YAG laser provided that such treatment would increase the surface roughness followed improved adhesion of hydroxyapatite (HAp) coatings The hydroxyapatite was deposited by electrophoretic method in suspension of 0.5 g HA powder and 100 ml ethyl alcohol. The deposition was carried out for 10 min at 10 V voltage followed by drying at room temperature for 24 h and heating at 800°C for 1 h in vacuum. The thickness of the HAp coatings was found as of about 4.06 μm to 9.05 μm. The examinations of surfaces were carried out at each stage of the experiment with the ultra-high resolution scanning electron microscope. The measurements of surface roughness after laser treatment and after HAp deposition were performed with the Hommel Etamic Waveline profilograph.
PL
Dotychczasowe badania powierzchni wszczepów tytanowych dla chirurgii kostnej wykazały, że osteointegracja na powierzchniach rozwiniętych jest znacznie szybsza niż na powierzchniach gładkich, co za tym idzie chropowatość powierzchni implantu ma bardzo duży wpływ na adhezję składników środowiska biologicznego. W artykule przedstawiono wstępne wyniki badań dotyczące wpływu chropowatości powierzchni stopu Ti13Nb13Zr o bardzo małym module Younga na budowę wytworzonej powłoki hydroksyapatytowej. Próbki z biostopu tytanu poddano obróbce laserowej za pomocą lasera Nd:YAG firmy Trumph o średniej mocy 150 W w celu zmiany geometrii powierzchni. Na tak przygotowanym podłożu wytwarzano powłoki hydroksyapatytowe metodą elektroforezy, stosując 0,5 i 1,0 g stężenie proszku HAp na 100 ml alkoholu etylowego. Osadzanie katodowe prowadzono przy napięciu 10 i 50 V przez 5 i 10 min. Po przeprowadzonej obróbce laserowej i wytworzeniu powłok HAp mierzono profil chropowatości powierzchni i prowadzono obserwacje za pomocą skaningowego mikroskopu elektronowego.
EN
So far research of the surfaces of titanium implants in bone surgery demonstrate that osteointegration on rough surface is much faster than on smooth ones. The roughness of implant surface influences then the adhesion of components of biological environment. In this paper the preliminary research results made on the Ti13Nb13Zr alloy treated with pulse laser and coated with hydroxyapatite are presented. The aim of the research was to determine the influence of effect of laser treatment and HAp deposition parameters on structure of the hydroxyapatite coating. The laser treatment was carried with the pulse Nd:YAG laser (Trumph) of the 150 W average power in order to change the surface geometry. Next the HAp coatings were deposited by electrophoretic method using the suspension of 0.5 or 1.0 g of HAp powder in 100 ml ethanol. The deposition was made at 10 V and 50 V for 5 and 10 min. The surface roughness profiles and microscopic examinations were performed after laser treatment and HAp deposition.
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