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- Residual strength (3)
- Atmospheric pressure plasma treatment (2)
- Femtosecond laser ablation (2)
- Fluorescence (2)
- Laser processing (2)
- Laser-induced periodic surface structures, LIPSS (2)
- Low pressure plasma pretreatment (2)
- Molecular orientation at polymer surfaces (2)
- Polyurethane-polypropylene adhesion (2)
- Quality assurance (2)
Organisationseinheit der BAM
The invention of new miniaturized and smart medical implants continues in all medical fields, including miniaturized heart pacemakers. These implants often come with a titanium (Ti) casing, which may have to be removed after several months or years and shall therefore not be completely overgrown by cells or scar tissue after implantation. Scar tissue is mainly formed by fibroblast cells and extracellular matrix proteins like collagen produced by them. Suppression of fibroblast growth at Ti surfaces could be achieved by 800 nm femtosecond laser-ablation creating self-organized sharp spikes with dimensions in the 10 μm-range which are superposed by fine sub-μm parallel ripples. On flat Ti control samples, the best results regarding suppression of cell growth were obtained on spike-structures which were additionally electrochemically anodized under acidic conditions. When Ti cylinders with a diameter of 8 mm (similar as the pacemakers) were placed upright in a culture of murine fibroblasts, a multi-layer cell growth up to a height of at least 1.5 mm occurred within 19–22 days. We have demonstrated that a laser-structured and anodized ring around the Ti cylinder surface is an effective way to create a barrier that murine fibroblasts were not able to overgrow within this time.
Herein, Ti6Al4V alloy is surface modified by femtosecond laser ablation. The microstructure image obtained by secondary electron microscopy reveals a combination of micrometer spikes or cones superimposed by nanoripples (laser‐induced periodic surface structures). To make the surface hydrophilic, anodization is performed resulting in further smoothness of microstructure and a final thickness of 35 ± 4 nm is estimated for oxide produced after anodization at 10 V (scan rate = 0.1 V s−1) versus standard hydrogen electrode. The obtained electrochemically active surface area (ECSA) is approximately 8 times larger compared with flat mirror polished Ti6Al4V surface. Combined chemical analysis by Pourbaix diagram and X‐ray photoelectron spectroscopy (XPS) analyses reveal that titanium and aluminum are passivating into TiO2 and Al2O3, but the dissolution of aluminum in the form of solvated ion is inevitable. Finally, cell seeding experiments on anodized and laser‐treated titanium alloy samples show that the growth of murine fibroblast cells is significantly suppressed due to unique surface texture of the laser‐treated and anodized titanium alloy sample.
Objective: The utilization of fluorescein-guided biopsies and resection has been recently discussed as a suitable strategy to improve and expedite operative techniques for the resection of central nervous system (CNS) tumors. However, little is known about the optical properties of sodium fluorescein (NaFl) in human tumor tissue and their potential impact on ex vivo analyses involving fluorescence-based methods.
Methods: Tumor tissue was obtained from a study cohort of an observational study on the utilization of fluorescein-guided biopsy and resection (n=5). The optical properties of fluorescein-stained tissue were compared to the optical features of the dye in vitro and in control samples consisting of tumor tissue of high-grade glioma patients (n=3) without intravenous (i.v.) application of NaFl. The dye-exposed tumor tissues were used for optical measurements to confirm the detectability of NaFl emission ex vivo. The tissue samples were fixed in 4%PFA, immersed in 30% sucrose, embedded in Tissue-Tek OCT compound, and cut to 10 mm cryosections. Spatially resolved emission spectra from tumor samples were recorded on representative slides with a Confocal Laser Scanning Microscope FV1000 (Olympus GmbH, Hamburg, Germany) upon excitation with lexc = 488 nm.
Results: Optical measurements of fluorescein in 0.9% sodium chloride (NaCl) under in vitro conditions showed an absorption maximum of lmax abs = 479 nm as detected with spectrophotometer Specord 200 and an emission peak at lmax em = 538 nm recorded with the emCCD detection system of a custom-made microscope-based single particle setup using a 500 nm long-pass filter. Further measurements revealed pH- and concentration-dependent emission spectra of NaFl. Under ex vivo conditions, confocal laser scanning microscopy of fluorescein tumor samples revealed a slight bathochromic shift and a broadening of the emission band.
Conclusion: Tumor uptake of NaFl leads to changes in the optical properties – a bathochromic shift and broadening of the emission band – possibly caused by the dye’s high pH sensitivity and concentration-dependent reabsorption acting as an innerfilter of the dye’s emission, particularly in the short wavelength region of the Emission spectrum where absorption and fluorescence overlap. Understanding the ex vivo optical properties of fluorescein is crucial for testing and validating its further applicability as an optical probe for intravital microscopy, immunofluorescence localization studies, and flow cytometry analysis.
Faserverbundwerkstoffe (Komposite) zeigen außergewöhnliche Veränderungen ihrer Eigenschaften in Abhängigkeit von der Betriebsdauer. Daraus leitet sich auch die Notwendigkeit ab, eine Methode zu finden, die in der Lage ist, Festigkeiten und Restfestigkeiten von Komposit-Druckbehältern zu ermitteln. Dies kann mittels Lastwechselprüfung oder in anderen Fällen vorzugsweise mittels der langsamen Berstprüfung erfolgen. Für eine aussagekräftige Beschreibung der Festigkeit bedürfen die Ergebnisse beider Prüfverfahren einer statistischen Auswertung. Aber insbesondere die statistische Auswertung der berstbezogenen Festigkeitseigenschaften unterliegt neben der Frage der Stichprobengröße einer großen Unsicherheit mit enormen Folgen. Dies ist die Frage, welche Verteilungsfunktion der Streuung der Festigkeitseigenschaft konservativ zugrundegelegt werden darf. So ist zu untersuchen, ob die Gaußsche Normalverteilung (NV) die wahre Verteilung richtig beschreibt. Es könnten aber auch andere Funktionen, wie z. B. die Weibull-Verteilung notwendig sein, um eine Überschätzung der Überlebenswahrscheinlichkeit bzw. Zuverlässigkeit in dem interessanten Bereich von einem Ausfall pro 104 bis 108 Druckbehältern zu vermeiden.
Slow burst testing of samples as a method for quantification of composite cylinder degradation
(2014)
The current practise to focus periodic retesting of composite cylinders primarily on the hydraulic pressure test has to be evaluated as critical. The test itself always causes a certain amount of micro damage to the cylinders but does not necessarily deliver sufficient and evaluable information. Thus BAM Federal Institute of Materials Research and Testing (Germany) moves the focal point to a new approach for validation of composite cylinders, based on destructive sample tests parallel to operation. Statistical assessment of results of these destructive tests is employed for the estimation of remaining safe service life, based on reliability demands. The estimated service life is also used for the determination of re-test periods of the examined population of composite cylinders.
An essential aspect of this approach is the validation of current residual strength and its prediction at any point of service life. In cases of gas cylinders with very high cycle strength, residual strength cannot be quantified statistically by means of hydraulic load cycles. As a replacement, creep tests or burst tests may be employed. BAM suggests the 'slow burst test SBT' as a combination of these two test procedures. This is a compromise between the practicability of the (conventional) burst test and the practical relevance of sustained loads during service, to be tested in creep rupture tests. In this paper, a variety of 99 burst results of a cylinder design type used for breathing apparatus (CFRP with PE-liner) is evaluated. The influence of test procedure parameters and nature and intensity of artificial ageing on the test sample strength are analysed statistically. This leads to an evaluation of different procedures of artificial ageing and the recommendation to substitute conventional burst tests by slow burst tests for the assessment of composite pressure receptacles.
There is evidence that composite materials degrade under static loads. Consequently there is no way to design composite gas cylinders for unlimited service life. Yet this fact is not reflected by design standards for composite receptacles approved for the transport of dangerous goods or for stationary application. Unnecessary cost and weight result from this.
Due to the degradation aspects of composites it is necessary to provide appropriate retesting procedures, which allow rejection of used vessels as is common practice for metallic receptacles. The current procedure of hydraulic tests appears to be an expensive procedure with serious doubts regarding its usefulness for composite cylinders.
Consequently, an efficient method is needed, which allows limiting the life time to its safe maximum. It is thus recommended to combine retesting with the assessment of residual life time. Since relevant non-destructive methods are not yet sufficiently matured and standardized enough, a concept featuring destructive tests on composite cylinders parallel to operation should be considered. An alternative concept introduced here, proposes to substitute the hydraulic testing of 100% of a population by a probabilistic evaluation of destructive tests on samples parallel to operation. Intensified pre-fill inspections should be an additional component of such a concept.