scholarly journals Correlative Microscopy Study of FIB Patterned Stainless Steel Surfaces as Novel Nano-Structured Stents for Cardiovascular Applications

2012 ◽  
Vol 1466 ◽  
Author(s):  
Michael Schmidt ◽  
Feroze Nazneen ◽  
Gregoire Herzog ◽  
Damien Arrigan ◽  
Paul Galvin ◽  
...  

ABSTRACTCoronary artery disease is a major problem worldwide causing 7.2 million deaths worldwide annually, resulting from vascular occlusion, myocardial infarction and its complications. Stent implantation is a percutaneous interventional procedure that mitigates vessel stenosis, providing mechanical support within the artery. However, stenting causes physical damage to the arterial wall. It is well accepted that a valuable route to reduce in-stent re-stenosis can be based on promoting cell response to nano-structured stainless steel (SS) surfaces such as, for example, by patterning nano-pits in SS. In this regard patterning by Focussed Ion-Beam (FIB) milling offers several advantages for flexible prototyping (i) practically any substrate material that is able to withstand high vacuum conditions of the microscope chamber can be used, (ii) there is high flexibility in the obtainable shapes and geometries by modulating the ion beam current and the patterning conditions, (iii) reduced complexity of the pattering process e.g. it is a single-step process with a possibility of real-time monitoring of the milling progression. On the other hand FIB patterning of polycrystalline metals is greatly influenced by channelling effects and re-deposition. Correlative microscopy methods present an opportunity to study such effects comprehensively and derive structure-property understanding that is important for developing improved pattering. In this report we present a FIB patterning protocol for nano-structuring features (concaves) ordered in rectangular arrays on pre-polished 316L Stainless Steel (SS) surfaces. An investigation based on correlative microscopy approach of the size, shape and depth of the developed arrays in relation to the crystal orientation of the underlying SS domains, is presented. The correlative microscopy protocol is based on cross-correlation of top-view Scanning Electron Microscopy (SEM), Electron Backscattered Diffraction (EBSD), and Atomic Force Microscopy (AFM).Various dose tests were performed, aiming at improved productivity by preserving nano-size accuracy of the patterned process. The optimal FIB patterning conditions for achieving reasonably high throughput (patterned rate of about 0.03 mm2 per hour) and nano-size accuracy in dimensions and shapes of the features, are discussed as well.

Author(s):  
Bilal Rasul ◽  
Hira Naz

We have performed surface-induced dissociation studies of small deuterated hydrocarbon cations i.e. CDx+ with x=2-4, colliding with two types of tungsten-coated surfaces, in the incident energy range between Ein = 0 eV approximately, up to Ein = 100 eV. A 34 nm thick W layer deposited on stainless steel using the Thermionic Vacuum Arc (TVA) method and a small sample of a tile cut from ASDEX-Upgrade tiles, consisting of PlasmaSprayed (PS) tungsten on carbon, are exposed to ion flux in these experiments. A double-focussing reverse geometry BE mass spectrometer, is used under ultra high vacuum conditions. Mass spectra of secondary charged particles are recorded via time-of-flight mass analyser. For comparison, we have performed equivalent study on polished stainless steel under experimental status explained in Section 2 below. At very low energies i.e. below 10 eV, only surface reflected projectiles are seen, whereas most of them are neutralized by surface micro charges. We observed that the fragmentation pattern of the small molecular ions at a given energy is strongly dependent on the surface. The roughness of both of the said thin films and their reflectivity for the projectile ion beam is studied by analysis of the ion yields of the reaction products


Author(s):  
K. N. Hooghan ◽  
K. S. Wills ◽  
P.A. Rodriguez ◽  
S.J. O’Connell

Abstract Device repair using Focused Ion Beam(FIB) systems has been in use for most of the last decade. Most of this has been done by people who have been essentially self-taught. The result has been a long learning curve to become proficient in device repair. Since a great deal of the problem is that documentation on this “art form” is found in papers from many different disciplines, this work attempts to summarize all of the available information under one title. The primary focus of FIB device repair is to ensure and maintain device integrity and subsequently retain market share while optimizing the use of the instrument, usually referred to as ‘beam time’. We describe and discuss several methods of optimizing beam time. First, beam time should be minimized while doing on chip navigation to reach the target areas. Several different approaches are discussed: dead reckoning, 3-point alignment, CAD-based navigation, and optical overlay. Second, after the repair areas are located and identified, the desired metal levels must be reached using a combination of beam currents and gas chemistries, and then filled up and strapped to make final connections. Third, cuts and cleanups must be performed as required for the final repair. We will discuss typical values of the beam currents required to maintain device integrity while concurrently optimizing repair time. Maintaining device integrity is difficult because of two potentially serious interactions of the FIB on the substrate: 1) since the beam consists of heavy metal ions (typically Gallium) the act of imaging the surface produces some physical damage; 2) the beam is positively charged and puts some charge into the substrate, making it necessary to use great care working in and around capacitors or active areas such as transistors, in order to avoid changing the threshold voltage of the devices. Strategies for minimizing potential damage and maximizing quality and throughput will be discussed.


Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 3048
Author(s):  
Rok Podlipec ◽  
Esther Punzón-Quijorna ◽  
Luka Pirker ◽  
Mitja Kelemen ◽  
Primož Vavpetič ◽  
...  

The metallic-associated adverse local tissue reactions (ALTR) and events accompanying worn-broken implant materials are still poorly understood on the subcellular and molecular level. Current immunohistochemical techniques lack spatial resolution and chemical sensitivity to investigate causal relations between material and biological response on submicron and even nanoscale. In our study, new insights of titanium alloy debris-tissue interaction were revealed by the implementation of label-free high-resolution correlative microscopy approaches. We have successfully characterized its chemical and biological impact on the periprosthetic tissue obtained at revision surgery of a fractured titanium-alloy modular neck of a patient with hip osteoarthritis. We applied a combination of photon, electron and ion beam micro-spectroscopy techniques, including hybrid optical fluorescence and reflectance micro-spectroscopy, scanning electron microscopy (SEM), Energy-dispersive X-ray Spectroscopy (EDS), helium ion microscopy (HIM) and micro-particle-induced X-ray emission (micro-PIXE). Micron-sized wear debris were found as the main cause of the tissue oxidative stress exhibited through lipopigments accumulation in the nearby lysosome. This may explain the indications of chronic inflammation from prior histologic examination. Furthermore, insights on extensive fretting and corrosion of the debris on nm scale and a quantitative measure of significant Al and V release into the tissue together with hydroxyapatite-like layer formation particularly bound to the regions with the highest Al content were revealed. The functional and structural information obtained at molecular and subcellular level contributes to a better understanding of the macroscopic inflammatory processes observed in the tissue level. The established label-free correlative microscopy approach can efficiently be adopted to study any other clinical cases related to ALTR.


1996 ◽  
Vol 438 ◽  
Author(s):  
N. Tsubouchi ◽  
Y. Horino ◽  
B. Enders ◽  
A. Chayahara ◽  
A. Kinomura ◽  
...  

AbstractUsing a newly developed ion beam apparatus, PANDA (Positive And Negative ions Deposition Apparatus), carbon nitride films were prepared by simultaneous deposition of mass-analyzed low energy positive and negative ions such as C2-, N+, under ultra high vacuum conditions, in the order of 10−6 Pa on silicon wafer. The ion energy was varied from 50 to 400 eV. The film properties as a function of their beam energy were evaluated by Rutherford Backscattering Spectrometry (RBS), Fourier Transform Infrared spectroscopy (FTIR) and Raman scattering. From the results, it is suggested that the C-N triple bond contents in films depends on nitrogen ion energy.


1996 ◽  
Vol 438 ◽  
Author(s):  
R. L. C. Wu ◽  
W. Lanter

AbstractAn ultra high vacuum ion beam system, consisting of a 20 cm diameter Rf excilted (13.56 MHz) ion gun and a four-axis substrate scanner, has been used to modify large surfaces (up to 1000 cm2) of various materials, including; infrared windows, silicon nitride, polycrystalline diamond, 304 and 316 stainless steels, 440C and M50 steels, aluminum alloys, and polycarbonates; by depositing different chemical compositions of diamond-like carbon films. The influences of ion energy, Rf power, gas composition (H2/CH4 , Ar/CH4 and O2/CH4/H2), on the diamond-like carbon characteristics has been studied. Particular attention was focused on adhesion, environmental effects, IR(3–12 μm) transmission, coefficient of friction, and wear factors under spacelike environments of diamond-like carbon films on various substrates. A quadrupole mass spectrometer was utilized to monitor the ion beam composition for quality control and process optimization.


2017 ◽  
Vol 24 (03) ◽  
pp. 1750038 ◽  
Author(s):  
A. M. ABDEL REHEEM ◽  
A. ATTA ◽  
T. A. AFIFY

In this work, PVA/Ag nanocomposites films were prepared using solution casting technique, these films were irradiated with Argon ion beam to modify the structure. The main objective of the study is to enhance the optical and electrical properties of the polymer nanocomposites films by irradiation. The conventional characterization techniques such as UV–Visible spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR), transmission electron microscope (TEM) and dielectric measurement are employed to understand the structure–property relations. FTIR analysis of these composite films shows chemical changes and a significant impact on them can be observed after irradiation. After doping, the XRD data shows silver nanoparticles formation in the PVA polymer. The band gap energy of samples is decreased with increases in the concentration of silver nanoparticles and ion beam fluence, which gives clear indication that ion beam irradiation induced defects are formed in the composite systems. The electrical conductivity, dielectric loss [Formula: see text] and dielectric constant [Formula: see text] are increased with increasing ion beam fluence and Ag dopant concentration.


Metals ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 208 ◽  
Author(s):  
Xinchun Chen ◽  
Xuan Yin ◽  
Jie Jin

To satisfy the harsh service demand of stainless steel and aviation bearing steel, the anticorrosion and wettability behaviors of 9Cr18 stainless steel and M50 bearing steel tailored by ion beam surface modification technology were experimentally investigated. By controlling the ion implantation (F+, N+, N+ + Ti+) or deposition processes, different surface-modified layers and ceramic layers or composite layers with both effects (ion implantation and deposition processes) were obtained on metal surfaces. The wettability was characterized by a contact angle instrument, and the thermodynamics stabilization of ion implantation-treated metals in corrosive solution was evaluated through an electrochemical technique. X-ray photoelectron spectroscopy (XPS) was employed for detecting the chemical bonding states of the implanted elements. The results indicated that ion implantation or deposition-induced surface-modified layers or coating layers could increase water contact angles, namely improving hydrophobicity as well as thermodynamic stabilization in corrosive medium. Meanwhile, wettability with lubricant oil was almost not changed. The implanted elements could induce the formation of new phases in the near-surface region of metals, and the wettability behaviors were closely related to the as-formed ceramic components and amorphous sublayer.


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