scholarly journals Preparation of Metal Nitride Particles Using Arc Discharge in Liquid Nitrogen

Nanomaterials ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 2214
Author(s):  
Yoon Sik Park ◽  
Satoshi Kodama ◽  
Hidetoshi Sekiguchi

A simple process to synthesize metal nitride particles was proposed using submerged arc discharge plasma in liquid nitrogen. Gibbs standard free energy was considered for the selection of the nitride-forming materials. In this study, titanium (Ti) and aluminum (Al) electrodes were used as raw materials for nitride particle preparation. Liquid nitrogen acted as a dielectric medium as well as a nitridation source in this process. A copper electrode was also used as a non-reactive material for comparison with the reactive Ti and Al electrodes. As the operating conditions of the experiments, the arc discharge current was varied from 5 A (low-power mode) to 30 A (high-power mode). The formation of titanium nitride (TiN) and aluminum nitride (AlN) was confirmed in the particles prepared in all experimental conditions by X-ray powder diffraction (XRD). The observation using a field emission scanning electron microscope (FE-SEM) and a field emission transmission electron microscope (FE-TEM) indicated that the synthesized TiN particles showed a cubic morphology, whereas AlN particles containing unreacted Al showed a spherical morphology. The experiments using different metal electrode configurations showed that the anode generated most of the particles in this process. Based on the obtained results, a particle formation mechanism was proposed.

Author(s):  
M. Iwatsuki ◽  
Y. Kokubo ◽  
Y. Harada

On accout of its high brightness, small optical source size, and minimal energy spread, the field emission gun (FEG) has the advantage that it provides the conventional transmission electron microscope (TEM) with a highly coherent illumination system and directly improves the resolving power and signal-to-noise ratio of the scanning electron microscope (SEM). The FEG is generally classified into two types; the cold field emission (C-FEG) and thermal field emission gun (T-FEG). The former, in which a field emitter is used at the room temperature, was successfully developed as an electron source for the SEM. The latter, in which the emitter is heated to the temperature range of 1000-1800°K, was also proved to be very suited as an electron source for the TEM, as well as for the SEM. Some characteristics of the two types of the FEG have been studied and reported by many authors. However, the results of the respective types have been obtained separately under different experimental conditions.


Author(s):  
S. Saito ◽  
Y. Nakaizumi ◽  
T. Nagatani ◽  
H. Todokoro

We have developed an ultra high resolution scanning electron mícroscope utílízíng a fíeld emíssíon electron source (Fig.1). This instrument has a guaranteed resolution of 2 nm in the secondary electron image mode and it has incorporated a microprocessor control for optimized operating conditions and maximum ease of operation by various automated functions. The microprocessor control system includes field emission electron gun control, electron optical system control, and video signal control. The field emission electron gun control system includes flashing operation which is used to clean the tip surface by heating for a very short time, high voltage operation of accelerating voltage (V0) and tip voltage (V1), correction of emission current which changes with time, and correction of virtual source position which changes with a voltage ratio V0/V1. We have automated these series of operations by developing an auto FE gun control system. Fig. 2 shows details of this system.


CONVERTER ◽  
2021 ◽  
pp. 176-189
Author(s):  
Jiangchun Li, Et al.

Objectives: Paper documents are playing an increasingly important role in people's daily work with the development of economy, society and culture. In the practice of judicial appraisal, the sequence of the intersections of ink and seal on suspicious documents can often provide critical information for the detection of criminal cases. The examination of sequence of intersecting seal and ink lines is to judge the sequence of seal and ink mark formation by certain technical means.Methods: A representative black signature pen, ink, and specific paper are selected to prepare experimental samples. Under the given experimental conditions, the field emission scanning electron microscope is used to perform micro-morphology on the cross-sectional characteristics of the samples and all the characterization results obtained are systematically analyzed to summarize the specificity of the sample. Results: The results showed that the proposed method can efficiently discriminate the Permeation Characterization of the sequence of intersecting seal and ink lines.Conclusions: This research is expected to be applied to forensic investigation for counterfeiting documents and bring new developments in the field of document inspection.


Author(s):  
Louis T. Germinario

A liquid nitrogen stage has been developed for the JEOL JEM-100B electron microscope equipped with a scanning attachment. The design is a modification of the standard JEM-100B SEM specimen holder with specimen cooling to any temperatures In the range ~ 55°K to room temperature. Since the specimen plane is maintained at the ‘high resolution’ focal position of the objective lens and ‘bumping’ and thermal drift la minimized by supercooling the liquid nitrogen, the high resolution capability of the microscope is maintained (Fig.4).


Author(s):  
S. Saito ◽  
H. Todokoro ◽  
S. Nomura ◽  
T. Komoda

Field emission scanning electron microscope (FESEM) features extremely high resolution images, and offers many valuable information. But, for a specimen which gives low contrast images, lateral stripes appear in images. These stripes are resulted from signal fluctuations caused by probe current noises. In order to obtain good images without stripes, the fluctuations should be less than 1%, especially for low contrast images. For this purpose, the authors realized a noise compensator, and applied this to the FESEM.Fig. 1 shows an outline of FESEM equipped with a noise compensator. Two apertures are provided gust under the field emission gun.


Author(s):  
Michel Troyonal ◽  
Huei Pei Kuoal ◽  
Benjamin M. Siegelal

A field emission system for our experimental ultra high vacuum electron microscope has been designed, constructed and tested. The electron optical system is based on the prototype whose performance has already been reported. A cross-sectional schematic illustrating the field emission source, preaccelerator lens and accelerator is given in Fig. 1. This field emission system is designed to be used with an electron microscope operated at 100-150kV in the conventional transmission mode. The electron optical system used to control the imaging of the field emission beam on the specimen consists of a weak condenser lens and the pre-field of a strong objective lens. The pre-accelerator lens is an einzel lens and is operated together with the accelerator in the constant angular magnification mode (CAM).


Author(s):  
N. Tamura ◽  
T. Goto ◽  
Y. Harada

On account of its high brightness, the field emission electron source has the advantage that it provides the conventional electron microscope with highly coherent illuminating system and that it directly improves the, resolving power of the scanning electron microscope. The present authors have reported some results obtained with a 100 kV field emission electron microscope.It has been proven, furthermore, that the tungsten emitter as a temperature field emission source can be utilized with a sufficient stability under a modest vacuum of 10-8 ~ 10-9 Torr. The present paper is concerned with an extension of our study on the characteristics of the temperature field emitters.


Author(s):  
M.K. Lamvik ◽  
D.A. Kopf ◽  
S.D. Davilla ◽  
J.D. Robertson

Last year we reported1 that there is a striking reduction in the rate of mass loss when a specimen is observed at liquid helium temperature. It is important to determine whether liquid helium temperature is significantly better than liquid nitrogen temperature. This requires a good understanding of mass loss effects in cold stages around 100K.


Author(s):  
Vinayak P. Dravid ◽  
H. Zhang ◽  
L.D. Marks ◽  
J.P. Zhang

A 200 kV cold field emission gun atomic resolution analytical electron microscope (ARAEM, Hitachi HF-2000) has been recently installed at Northwestern. The ARAEM offers an unprecedented combination of atomic structure imaging of better than 0.20 nm nominal point-to-point resolution and about 0.10 nm line resolution, alongwith nanoscale analytical capabilities and electron holography in one single instrument. The ARAEM has been fully functional/operational and this paper presents some illustrative examples of application of ARAEM techniques to oxide superconductors. Additional results will be presented at the meeting.


Author(s):  
B.G. Frost ◽  
D.C. Joy ◽  
L.F. Allard ◽  
E. Voelkl

A wide holographic field of view (up to 15 μm in the Hitachi-HF2000) is achieved in a TEM by switching off the objective lens and imaging the sample by the first intermediate lens. Fig.1 shows the corresponding ray diagram for low magnification image plane off-axis holography. A coherent electron beam modulated by the sample in its amplitude and its phase is superimposed on a plane reference wave by a negatively biased Möllenstedt-type biprism.Our holograms are acquired utilizing a Hitachi HF-2000 field emission electron microscope at 200 kV. Essential for holography are a field emission gun and an electron biprism. At low magnification, the excitation of each lens must be appropriately adjusted by the free lens control mode of the microscope. The holograms are acquired by a 1024 by 1024 slow-scan CCD-camera and processed by the “Holoworks” software. The hologram fringes indicate positively and negatively charged areas in a sample by the direction of the fringe bending (Fig.2).


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