scholarly journals Major Factors Influencing the Size Distribution Analysis of Cellulose Nanocrystals Imaged in Transmission Electron Microscopy

Polymers ◽  
2021 ◽  
Vol 13 (19) ◽  
pp. 3318
Author(s):  
Hui Qian

Size distributions of cellulose nanocrystals (CNCs), extracted from softwood pulp via strong sulfuric acid hydrolysis, exhibit large variability when analyzed from transmission electron microscopy (TEM) images. In this article, the causes of this variability are studied and discussed. In order to obtain results comparable with those reported, a reference material of CNCs (CNCD-1) was used to evaluate size distribution. CNC TEM specimens were prepared as-stained and dried with a rapid-flushing staining method or hydrated and embedded in vitreous ice with the plunge-freezing method. Several sets of bright-field TEM (BF-TEM), annular dark-field scanning TEM (ADF-STEM) and cryogenic-TEM (cryo-TEM) images were acquired for size distribution analysis to study the contributing factors. The rapid-flushing staining method was found to be the most effective for contrast enhancement of CNCs, not only revealing the helical structure of single CNCs but also resolving the laterally jointed CNCs. During TEM specimen preparation, CNCs were fractionated on TEM grids driven by the coffee-ring effect, as observed from contrast variation of CNCs with a stain-depth gradient. From the edge to the center of the TEM grids, the width of CNCs increases, while the aspect ratio (length to width) decreases. This fractionated dispersion of CNCs suggests that images taken near the center of a droplet would give a larger mean width. In addition to particle fractionation driven by the coffee-ring effect, the arrangement and orientation of CNC particles on the substrate significantly affect the size measurement when CNC aggregation cannot be resolved in images. The coexistence of asymmetric cross-section CNC particles introduces a large variation in size measurement, as TEM images of CNCs are mixed projections of the width and height of particles. As a demonstration of how this contributes to inflated size measurement, twisted CNC particles, rectangular cross-section particles and end-to-end jointed CNCs were revealed in reconstructed three-dimensional (3D) micrographs by electron tomography (ET).

Nanoscale ◽  
2015 ◽  
Vol 7 (48) ◽  
pp. 20593-20606 ◽  
Author(s):  
Martijn van Sebille ◽  
Laurens J. P. van der Maaten ◽  
Ling Xie ◽  
Karol Jarolimek ◽  
Rudi Santbergen ◽  
...  

We propose a method to quickly detect and measure the nanocrystal size distribution from TEM images.


1997 ◽  
Vol 36 (4) ◽  
pp. 313-320 ◽  
Author(s):  
D. Snidaro ◽  
F. Zartarian ◽  
F. Jorand ◽  
J.-Y. Bottero ◽  
J.-C. Block ◽  
...  

Activated sludge is the most widely used process for wastewater treatment. However basic properties such as floc structure or settling properties, still remain unknown. In order to describe activated sludge floc structure, four investigation methods were used: (i) size distribution analysis associated with sonication, (ii) transmission electron microscopy (iii) laser scanning confocal microscopy and fractal dimension analysis, and (iv) three dimensional modelling. The evolution of floc size distribution in dispersed samples was used to build a model of floc showing that the predominating microflocs (125 μm) are formed from 13 μm aggregates, which are made up of smaller particles (2.5 μm). By transmission electron microscopy it was assumed that the 2.5 μm sub-units could correspond to microorganisms and that exopolymers form a gel-like matrix which holds the structure of the aggregates together. The microfloc (13 μm) structure was investigated by confocal scanning light microscopy and image processing. The analysis of the mass distribution pointed out that the microfloc is a fractal object (fractal dimension around 3). The total number of cells in these aggregates was found to be 2n number. These two results suggest that division of microorganisms explained the formation of 13 μm units which are microcolonies. A mass fractal dimension 2.5 ± 0.15 was measured for the microfloc. Its external surface was reconstructed by using interpolating software (GOCAD). It appeared that the surface is also a fractal object with a dimension 2.3 ± 0.1. According to the fractal theory, it seems that diffusion limited aggregation via monomer-cluster collision is the mechanism which describes the formation of macroflocs.


Author(s):  
D. L. Callahan ◽  
Z. Ball ◽  
H. M. Phillips ◽  
R. Sauerbrey

Ultraviolet laser-irradiation can be used to induce an insulator-to-conductor phase transition on the surface of Kapton polyimide. Such structures have potential applications as resistors or conductors for VLSI applications as well as general utility electrodes. Although the percolative nature of the phase transformation has been well-established, there has been little definitive work on the mechanism or extent of transformation. In particular, there has been considerable debate about whether or not the transition is primarily photothermal in nature, as we propose, or photochemical. In this study, cross-sectional optical microscopy and transmission electron microscopy are utilized to characterize the nature of microstructural changes associated with the laser-induced pyrolysis of polyimide.Laser-modified polyimide samples initially 12 μm thick were prepared in cross-section by standard ultramicrotomy. Resulting contraction in parallel to the film surface has led to distortions in apparent magnification. The scale bars shown are calibrated for the direction normal to the film surface only.


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.


Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 2849
Author(s):  
Marcin Jan Dośpiał

This paper presents domain and structure studies of bonded magnets made from nanocrystalline Nd-(Fe, Co)-B powder. The structure studies were investigated using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Mössbauer spectroscopy and X-ray diffractometry. On the basis of performed qualitative and quantitative phase composition studies, it was found that investigated alloy was mainly composed of Nd2(Fe-Co)14B hard magnetic phase (98 vol%) and a small amount of Nd1.1Fe4B4 paramagnetic phase (2 vol%). The best fit of grain size distribution was achieved for the lognormal function. The mean grain size determined from transmission electron microscopy (TEM) images on the basis of grain size distribution and diffraction pattern using the Bragg equation was about ≈130 nm. HRTEM images showed that over-stoichiometric Nd was mainly distributed on the grain boundaries as a thin amorphous border of 2 nm in width. The domain structure was investigated using a scanning electron microscope and metallographic light microscope, respectively, by Bitter and Kerr methods, and by magnetic force microscopy. Domain structure studies revealed that the observed domain structure had a labyrinth shape, which is typically observed in magnets, where strong exchange interactions between grains are present. The analysis of the domain structure in different states of magnetization revealed the dynamics of the reversal magnetization process.


2010 ◽  
Vol 16 (6) ◽  
pp. 662-669 ◽  
Author(s):  
S. Simões ◽  
F. Viana ◽  
A.S. Ramos ◽  
M.T. Vieira ◽  
M.F. Vieira

AbstractReactive multilayer thin films that undergo highly exothermic reactions are attractive choices for applications in ignition, propulsion, and joining systems. Ni/Al reactive multilayer thin films were deposited by dc magnetron sputtering with a period of 14 nm. The microstructure of the as-deposited and heat-treated Ni/Al multilayers was studied by transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) in plan view and in cross section. The cross-section samples for TEM and STEM were prepared by focused ion beam lift-out technique. TEM analysis indicates that the as-deposited samples were composed of Ni and Al. High-resolution TEM images reveal the presence of NiAl in small localized regions. Microstructural characterization shows that heat treating at 450 and 700°C transforms the Ni/Al multilayered structure into equiaxed NiAl fine grains.


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