scholarly journals Precipitation of Pt Nanoparticles inside Ion-Track-Etched Capillaries

2020 ◽  
Vol 4 (1) ◽  
pp. 8 ◽  
Author(s):  
Shunya Yamamoto ◽  
Hiroshi Koshikawa ◽  
Tomitsugu Taguchi ◽  
Tetsuya Yamaki

Ion-track-etched capillaries containing nanoparticles of precious metals (e.g., Pt, Au, and Ag) can be applied to plasmonic absorber materials. The precipitation of homogeneous and highly dispersed precious metal nanoparticles inside capillaries represents a key process. Ion-track-etched capillaries (diameter: ~500 nm, length: ~25 μm) were created in polyimide film by 350 MeV Xe irradiation (3 × 107 ions/cm2) and chemical etching (using a sodium hypochlorite solution). The films with capillaries were immersed in an aqueous solution containing 0.1–10 mmol/L H2PtCl6 and 0.5 vol% C2H5OH, and then irradiated with a 2 MeV electron beam up to a fluence of 1.4 × 1016 e/cm2. The Pt particles inside the capillaries were characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The precipitation of Pt nanoparticles and isolated aggregates inside the capillaries was confirmed by TEM. The Pt nanoparticles tended to aggregate under increasing concentrations of H2PtCl6 in the aqueous solution; meanwhile, no changes in nanoparticle size were noted under increasing electron beam fluence. The results suggest that the proposed method can be used to form metal nanoparticles in nanosized capillaries with a high aspect ratio.

Author(s):  
G. G. Shaw

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.


Author(s):  
Joseph J. Comer ◽  
Charles Bergeron ◽  
Lester F. Lowe

Using a Van De Graaff Accelerator thinned specimens were subjected to bombardment by 3 MeV N+ ions to fluences ranging from 4x1013 to 2x1016 ions/cm2. They were then examined by transmission electron microscopy and reflection electron diffraction using a 100 KV electron beam.At the lowest fluence of 4x1013 ions/cm2 diffraction patterns of the specimens contained Kikuchi lines which appeared somewhat broader and more diffuse than those obtained on unirradiated material. No damage could be detected by transmission electron microscopy in unannealed specimens. However, Dauphiné twinning was particularly pronounced after heating to 665°C for one hour and cooling to room temperature. The twins, seen in Fig. 1, were often less than .25 μm in size, smaller than those formed in unirradiated material and present in greater number. The results are in agreement with earlier observations on the effect of electron beam damage on Dauphiné twinning.


Author(s):  
Marc J.C. de Jong ◽  
Wim M. Busing ◽  
Max T. Otten

Biological materials damage rapidly in the electron beam, limiting the amount of information that can be obtained in the transmission electron microscope. The discovery that observation at cryo temperatures strongly reduces beam damage (in addition to making it unnecessaiy to use chemical fixatives, dehydration agents and stains, which introduce artefacts) has given an important step forward to preserving the ‘live’ situation and makes it possible to study the relation between function, chemical composition and morphology.Among the many cryo-applications, the most challenging is perhaps the determination of the atomic structure. Henderson and co-workers were able to determine the structure of the purple membrane by electron crystallography, providing an understanding of the membrane's working as a proton pump. As far as understood at present, the main stumbling block in achieving high resolution appears to be a random movement of atoms or molecules in the specimen within a fraction of a second after exposure to the electron beam, which destroys the highest-resolution detail sought.


Author(s):  
L. D. Peachey ◽  
J. P. Heath ◽  
G. Lamprecht

Biological specimens of cells and tissues generally are considerably thicker than ideal for high resolution transmission electron microscopy. Actual image resolution achieved is limited by chromatic aberration in the image forming electron lenses combined with significant energy loss in the electron beam due to inelastic scattering in the specimen. Increased accelerating voltages (HVEM, IVEM) have been used to reduce the adverse effects of chromatic aberration by decreasing the electron scattering cross-section of the elements in the specimen and by increasing the incident electron energy.


Author(s):  
B. L. Armbruster ◽  
B. Kraus ◽  
M. Pan

One goal in electron microscopy of biological specimens is to improve the quality of data to equal the resolution capabilities of modem transmission electron microscopes. Radiation damage and beam- induced movement caused by charging of the sample, low image contrast at high resolution, and sensitivity to external vibration and drift in side entry specimen holders limit the effective resolution one can achieve. Several methods have been developed to address these limitations: cryomethods are widely employed to preserve and stabilize specimens against some of the adverse effects of the vacuum and electron beam irradiation, spot-scan imaging reduces charging and associated beam-induced movement, and energy-filtered imaging removes the “fog” caused by inelastic scattering of electrons which is particularly pronounced in thick specimens.Although most cryoholders can easily achieve a 3.4Å resolution specification, information perpendicular to the goniometer axis may be degraded due to vibration. Absolute drift after mechanical and thermal equilibration as well as drift after movement of a holder may cause loss of resolution in any direction.


Author(s):  
H.J. Ryu ◽  
A.B. Shah ◽  
Y. Wang ◽  
W.-H. Chuang ◽  
T. Tong

Abstract When failure analysis is performed on a circuit composed of FinFETs, the degree of defect isolation, in some cases, requires isolation to the fin level inside the problematic FinFET for complete understanding of root cause. This work shows successful application of electron beam alteration of current flow combined with nanoprobing for precise isolation of a defect down to fin level. To understand the mechanism of the leakage, transmission electron microscopy (TEM) slice was made along the leaky drain contact (perpendicular to fin direction) by focused ion beam thinning and lift-out. TEM image shows contact and fin. Stacking fault was found in the body of the silicon fin highlighted by the technique described in this paper.


2015 ◽  
Author(s):  
Ludmila L. Meisner ◽  
Alexey A. Neiman ◽  
Alexander I. Lotkov ◽  
Nikolai N. Koval ◽  
Viktor O. Semin ◽  
...  

2012 ◽  
Vol 31 (4-5) ◽  
pp. 451-458 ◽  
Author(s):  
S. Fujieda ◽  
K. Shinoda ◽  
T. Inanaga ◽  
M. Abumiya ◽  
S. Suzuki

AbstractA novel process for preparing scorodite particles with a diameter of approximately 20 µm from Fe(II) and As(V) in aqueous solution has been developed by DOWA Metals and Mining. In the present study, the dissolution characteristics of iron and arsenic from the scorodite particles synthesized by this process have been investigated under different conditions. The results show that the concentration of arsenic dissolved from the particles in aqueous solution is very low, but it has a complicated dependence on the temperature and pH of the solution. Transmission electron microscopy (TEM) with an energy dispersive X-ray spectrometer (EDS) was used to analyze the morphology, structure, and composition of the scorodite particles. The results indicate that the scorodite particles exhibit a nearly octahedral shape with planes composed of almost (111) planes in the orthorhombic structure. The concentration of iron at the surface of the particles is higher than that of iron inside of the particles. This characteristic morphology, along with the minimal surface defects of the scorodite particles, is considered to be responsible for the low dissolution of arsenic from the particles in aqueous solution. Atmospheric temperature and solution conditions were also found to be important for the safe, long-term storage of arsenic using scorodite particles.


2013 ◽  
Vol 873 ◽  
pp. 206-210
Author(s):  
Kai Li ◽  
Rao Fu ◽  
Qing Ran Gao ◽  
Ai Wei Tang ◽  
Ying Feng Wang

This paper continues our previous work on preparation of triangular silver nanoparticles. The method proceeds with reaction of silver nitrate with hydrazine hydrate in the presence of polyvinyl pyrrolidone in aqueous solution. Effects of the concentration of PVP on the morphologies of Ag NPs were systematically investigated. The obtained Ag NPs were characterized by transmission electron microscopy and UV-visible spectrophotometer. The results showed that, triangular Ag NPs with edge lengths in the range of 50-200 nm were obtained using PVP as protective agent with lower concentration. As the concentration of PVP increased, spherical Ag NPs with their sizes about 6.2 nm were prepared and triangular Ag NPs were not obtained. The formation mechanism of triangular Ag NPs has been studied. Ostwald ripening is the driving force on the conversion of spherical Ag NPs to triangular Ag NPs in the presence of PVP.


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