In Situ Modification and Analysis of the Composition and Crystal Structure of a Silicon Target by Ion-Beam Methods

2018 ◽  
Vol 63 (12) ◽  
pp. 1861-1867 ◽  
Author(s):  
Yu. V. Balakshin ◽  
A. A. Shemukhin ◽  
A. V. Nazarov ◽  
A. V. Kozhemiako ◽  
V. S. Chernysh
2018 ◽  
Author(s):  
Xinmei Li ◽  
Shuangbo Zhang ◽  
Fei Sun

ABSTRACTMicroED (micro electron diffraction) is an emerging technique to use cryo-electron microscope to study the crystal structure of macromolecule from its micro/nano-crystals, which are not suitable for conventional X-ray crystallography. However, this technique has been prevented for its wide application by the limited availability of producing good micro-/nano-crystals and the inappropriate transfer of crystals. Here, we developed a complete workflow to prepare suitable crystals efficiently for MicroED experiment. This workflow includes in situ on-grid crystallization, single-side blotting, cryo-focus ion beam (cryo-FIB) fabrication, and cryo-electron diffraction of crystal cryo-lamella. This workflow enables us to apply MicroED to study many small macromolecular crystals with the size of 2 ~ 10 μm, which is too large for MicroED but quite small for conventional X-ray crystallography. We have applied this method to solve 2.5Å crystal structure of lysozyme from its micro-crystal within the size of 10×10×10 μm3. Our work will greatly expand the availability space of crystals suitable for MicroED and fill up the gap between MicroED and X-ray crystallography.


Author(s):  
J. S. Maa ◽  
Thos. E. Hutchinson

The growth of Ag films deposited on various substrate materials such as MoS2, mica, graphite, and MgO has been investigated extensively using the in situ electron microscopy technique. The three stages of film growth, namely, the nucleation, growth of islands followed by liquid-like coalescence have been observed in both the vacuum vapor deposited and ion beam sputtered thin films. The mechanisms of nucleation and growth of silver films formed by ion beam sputtering on the (111) plane of silicon comprise the subject of this paper. A novel mode of epitaxial growth is observed to that seen previously.The experimental arrangement for the present study is the same as previous experiments, and the preparation procedure for obtaining thin silicon substrate is presented in a separate paper.


Author(s):  
Dudley M. Sherman ◽  
Thos. E. Hutchinson

The in situ electron microscope technique has been shown to be a powerful method for investigating the nucleation and growth of thin films formed by vacuum vapor deposition. The nucleation and early stages of growth of metal deposits formed by ion beam sputter-deposition are now being studied by the in situ technique.A duoplasmatron ion source and lens assembly has been attached to one side of the universal chamber of an RCA EMU-4 microscope and a sputtering target inserted into the chamber from the opposite side. The material to be deposited, in disc form, is bonded to the end of an electrically isolated copper rod that has provisions for target water cooling. The ion beam is normal to the microscope electron beam and the target is placed adjacent to the electron beam above the specimen hot stage, as shown in Figure 1.


Author(s):  
A. K. Rai ◽  
R. S. Bhattacharya ◽  
M. H. Rashid

Ion beam mixing has recently been found to be an effective method of producing amorphous alloys in the binary metal systems where the two original constituent metals are of different crystal structure. The mechanism of ion beam mixing are not well understood yet. Several mechanisms have been proposed to account for the observed mixing phenomena. The first mechanism is enhanced diffusion due to defects created by the incoming ions. Second is the cascade mixing mechanism for which the kinematicel collisional models exist in the literature. Third mechanism is thermal spikes. In the present work we have studied the mixing efficiency and ion beam induced amorphisation of Ni-Ti system under high energy ion bombardment and the results are compared with collisional models. We have employed plan and x-sectional veiw TEM and RBS techniques in the present work.


Author(s):  
Charles W. Allen ◽  
Robert C. Birtcher

The uranium silicides, including U3Si, are under study as candidate low enrichment nuclear fuels. Ion beam simulations of the in-reactor behavior of such materials are performed because a similar damage structure can be produced in hours by energetic heavy ions which requires years in actual reactor tests. This contribution treats one aspect of the microstructural behavior of U3Si under high energy electron irradiation and low dose energetic heavy ion irradiation and is based on in situ experiments, performed at the HVEM-Tandem User Facility at Argonne National Laboratory. This Facility interfaces a 2 MV Tandem ion accelerator and a 0.6 MV ion implanter to a 1.2 MeV AEI high voltage electron microscope, which allows a wide variety of in situ ion beam experiments to be performed with simultaneous irradiation and electron microscopy or diffraction.At elevated temperatures, U3Si exhibits the ordered AuCu3 structure. On cooling below 1058 K, the intermetallic transforms, evidently martensitically, to a body-centered tetragonal structure (alternatively, the structure may be described as face-centered tetragonal, which would be fcc except for a 1 pet tetragonal distortion). Mechanical twinning accompanies the transformation; however, diferences between electron diffraction patterns from twinned and non-twinned martensite plates could not be distinguished.


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


2020 ◽  
Vol 35 (2) ◽  
pp. 221-228
Author(s):  
S.-B. Chen ◽  
T.-X. Li ◽  
S.-H. Wan ◽  
X. Huang ◽  
S.-W. Cai ◽  
...  

Author(s):  
Jian-Shing Luo ◽  
Hsiu Ting Lee

Abstract Several methods are used to invert samples 180 deg in a dual beam focused ion beam (FIB) system for backside milling by a specific in-situ lift out system or stages. However, most of those methods occupied too much time on FIB systems or requires a specific in-situ lift out system. This paper provides a novel transmission electron microscopy (TEM) sample preparation method to eliminate the curtain effect completely by a combination of backside milling and sample dicing with low cost and less FIB time. The procedures of the TEM pre-thinned sample preparation method using a combination of sample dicing and backside milling are described step by step. From the analysis results, the method has applied successfully to eliminate the curtain effect of dual beam FIB TEM samples for both random and site specific addresses.


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