Synthesis, microstructure and hardness of bulk ultrahard BN nanocomposites

2008 ◽  
Vol 23 (4) ◽  
pp. 981-993 ◽  
Author(s):  
D. Rafaja ◽  
V. Klemm ◽  
M. Motylenko ◽  
M.R. Schwarz ◽  
T. Barsukova ◽  
...  

Ultrahard boron nitride compacts containing nanosized domains of the cubic (c-BN), wurtzitic (w-BN), and hexagonal (h-BN) phase were synthesized at high-pressure/high-temperature (HP/HT) conditions. Hot-pressed and pyrolytic BN, both containing h-BN as a main component, were used as starting materials. The HP/HT products were investigated by x-ray diffraction via Rietveld and line-profile analysis, as well as high-resolution transmission electron microscopy. c-BN was the dominant phase in all products, complemented by up to 25 wt% w-BN and some remaining “compressed h-BN.” In particular samples, partial crystallographic coherence of adjacent crystallites to x-rays was observed, which has been previously found in superhard transition metal nitride-based nanocomposite coatings. In the BN nanocomposites, the partial coherence of nanocrystallites to x-rays was improved by their strong local preferred orientation, which is made possible by the well-known orientation relationships among h-BN, w-BN, and c-BN phases. The correlation between the weight fraction and the average size of the c-BN crystallites helped to describe the formation of c-BN/(w-BN) nanocomposites from submicron-sized h-BN domains in the starting materials. The Knoop and Vickers hardness of specimens with crystallite sizes ranging from 6 to ∼50 nm was found to be significantly higher than that of c-BN single crystals, despite the presence of residual h-BN.

2010 ◽  
Vol 129-131 ◽  
pp. 999-1003 ◽  
Author(s):  
Hendi Saryanto ◽  
S. Khaerudini Deni ◽  
Pudji Untoro ◽  
Mat Husin Saleh ◽  
Darwin Sebayang

The aim of this study is to determine the nanocrystalline size by using Williamson-Hall method of Fe80Cr20 powder which prepared by mechanical alloying process. X-rays diffraction line profile analysis was adopted to analyze the crystallite size and microstrains of Fe80Cr20 alloys powder. Transmission Electron Microscopy (TEM) was used to examine the microstructure morphology of the nanosized of Fe80Cr20 alloys. The crystallite size, microstrain, and lattice parameters were estimated by Williamson–Hall plot. The results showed that the mechanical alloying processes resulted the final product in nanocrystalline size range (below 12 nm) which confirmed by TEM observation and XRD line profile analysis.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Pierfrancesco Maltoni ◽  
Sergey A. Ivanov ◽  
Gianni Barucca ◽  
Gaspare Varvaro ◽  
Davide Peddis ◽  
...  

AbstractThe magnetic properties of SrFe12O19 (SFO) hard hexaferrites are governed by the complex relation to its microstructure, determining their relevance for permanent magnets´ applications. A set of SFO nanoparticles obtained by sol–gel self-combustion synthesis was selected for an in-depth structural X-Rays powder diffraction (XRPD) characterization by means of G(L) line-profile analysis. The obtained crystallites´ size distribution reveal a clear dependence of the size along the [001] direction on the synthesis approach, resulting in the formation of platelet-like crystallites. In addition, the size of the SFO nanoparticles was determined by transmission electron microscopy (TEM) analysis and the average number of crystallites within a particle was estimated. These results have been evaluated to illustrate the formation of single-domain state below a critical value, and the activation volume was derived from time dependent magnetization measurements, aiming to clarify the reversal magnetization process of hard magnetic materials.


2021 ◽  
Author(s):  
Pierfrancesco Maltoni ◽  
Sergey Alexander Ivanov ◽  
Gianni Barucca ◽  
Gaspare Varvaro ◽  
Davide Peddis ◽  
...  

Abstract The magnetic properties of SrFe12O19 (SFO) hard hexaferrites are governed by the complex relation to its microstructure, determining their relevance for permanent magnets´ applications. A set of SFO nanoparticles obtained by sol-gel self-combustion synthesis was selected for an in-depth structural X-Rays powder diffraction (XRPD) characterization by means of G(L) line-profile analysis. The obtained crystallites´ size distribution reveal a clear dependence of the size along the [001] direction on the synthesis approach, resulting in the formation of platelet-like crystallites. In addition, the size of the SFO nanoparticles was determined by transmission electron microscopy (TEM) analysis and the average number of crystallites within a particle was estimated. These results have been evaluated to illustrate the formation of single-domain state below a critical value, and the activation volume was derived from time dependent magnetization measurements, aiming to clarify the reversal magnetization process of hard magnetic materials.


2005 ◽  
Vol 20 (4) ◽  
pp. 366-375 ◽  
Author(s):  
T. Ungár ◽  
G. Tichy ◽  
J. Gubicza ◽  
R. J. Hellmig

Crystallite size determined by X-ray line profile analysis is often smaller than the grain or subgrain size obtained by transmission electron microscopy, especially when the material has been produced by plastic deformation. It is shown that besides differences in orientation between grains or subgrains, dipolar dislocation walls without differences in orientation also break down coherency of X-rays scattering. This means that the coherently scattering domain size provided by X-ray line profile analysis provides subgrain or cell size bounded by dislocation boundaries or dipolar walls.


2017 ◽  
Vol 899 ◽  
pp. 48-53
Author(s):  
Rodrigo Uchida Ichikawa ◽  
Walter Kenji Yoshito ◽  
Margarida Juri Saeki ◽  
Willian C.A. Maranhão ◽  
Fátima Goulart ◽  
...  

Nanostructured Mn-Zn ferrites were synthesized using co-precipitation in alkaline solution with different pH. The samples were characterized using X-ray diffraction (XRD), X-ray fluorescence (XRF), thermal analysis (TG-DTA), dynamic light scattering (DLS) and scanning electron microscopy (SEM) techniques. Monophasic nanoparticles were formed when synthesized with pH 10.5. This sample was heat-treated and its XRD data was refined by the Rietveld method. Mean crystallite sizes and microstrains were determined from X-ray line profile analysis using Single-Line and Warren-Averbach methods, which revealed a mean crystallite size of approximately 10 nm and negligible microstrains. Zn content was estimated using refined cell parameters, giving a value of 33 at %, in accordance with XRF result. TG-DTA revealed that the incorporation of α-Fe2O3 occurs around 1130 °C and 1200 °C with recrystallization of the Mn-Zn ferrite spinel phase. DLS showed that mean particle size increase with temperature up to 1159 nm at 800 °C. SEM analysis showed the samples agglomerate and present similar morphology with negligible size changing when calcined between 280 °C and 800 °C. However, the sample calcined at 1200 °C presents larger agglomerates due to the sintering process.


2006 ◽  
Vol 39 (1) ◽  
pp. 24-31 ◽  
Author(s):  
Paolo Scardi ◽  
Matteo Leoni

Powder diffraction data collected on a nanocrystalline ceria sample within a round robin conducted by the IUCr Commission on Powder Diffraction were analysed by two alternative approaches: (i) whole-powder-pattern modelling based upon a fundamental microstructural parameters approach, and (ii) a traditional whole-powder-pattern fitting followed by Williamson–Hall and Warren–Averbach analysis. While the former gives results in close agreement with those of transmission electron microscopy, the latter tends to overestimate the domain size effect, providing size values about 20% smaller. The origin of the discrepancy can be traced back to a substantial inadequacy of profile fitting with Voigt profiles, which leads to systematic errors in the following line profile analysis by traditional methods. However, independently of the model, those systematic errors seem to have little effect on the volume-weighted mean size.


2007 ◽  
Vol 22 (5) ◽  
pp. 1314-1321 ◽  
Author(s):  
J. Gubicza ◽  
S. Nauyoks ◽  
L. Balogh ◽  
J. Labar ◽  
T.W. Zerda ◽  
...  

Microstructure of sintered nanocrystalline SiC is studied by x-ray line profile analysis and transmission electron microscopy. The lattice defect structure and the crystallite size are determined as a function of pressure between 2 and 5.5 GPa for different sintering temperatures in the range from 1400 to 1800 °C. At a constant sintering temperature, the increase of pressure promotes crystallite growth. At 1800 °C when the pressure reaches 8 GPa, the increase of the crystallite size is impeded. The grain growth during sintering is accompanied by a decrease in the population of planar faults and an increase in the density of dislocations. A critical crystallite size above which dislocations are more abundant than planar defects is suggested.


2015 ◽  
Vol 48 (5) ◽  
pp. 1534-1542 ◽  
Author(s):  
Jose Solla-Gullon ◽  
Emmanuel Garnier ◽  
Juan M. Feliu ◽  
Matteo Leoni ◽  
Alberto Leonardi ◽  
...  

Pd nanocrystals were produced with uniform truncated-cube shape and a narrow size distribution, yielding controlled surface area fractions from low Miller index ({100}, {110}, {111}) crystalline facets. Details on the structure and morphology of the nanocrystals were obtained by combining X-ray powder diffraction line profile analysis, high-resolution transmission electron microscopy and surface electrochemistry based on Cu underpotential deposition.


2014 ◽  
Vol 47 (1) ◽  
pp. 303-315 ◽  
Author(s):  
Zhiyang Wang ◽  
Ulf Garbe ◽  
Huijun Li ◽  
Yanbo Wang ◽  
Andrew J. Studer ◽  
...  

This work presents a detailed microstructure and texture study of various hydrided Zircaloy-4 materials by neutron diffraction and microscopy. The results show that the precipitated δ-ZrH1.66generally follows the δ(111)//α(0001) and δ[1{\overline 1}0]//α[11{\overline 2}0] orientation relationship with the α-Zr matrix. The δ-hydride displays a weak texture that is determined by the texture of the α-Zr matrix, and this dependence essentially originates from the observed orientation correlation between α-Zr and δ-hydride. Neutron diffraction line profile analysis and high-resolution transmission electron microscopy observations reveal a significant number of dislocations present in the δ-hydride, with an estimated average density one order of magnitude higher than that in the α-Zr matrix, which contributes to the accommodation of the substantial misfit strains associated with hydride precipitation in the α-Zr matrix. The present observations provide an insight into the behaviour of δ-hydride precipitation in zirconium alloys and may help with understanding the induced embrittling effect of hydrides.


2016 ◽  
Vol 23 (5) ◽  
pp. 481-487 ◽  
Author(s):  
Pragyan Mohanty ◽  
Dilip Kumar Mishra ◽  
Shikha Varma ◽  
Kampal Mishra ◽  
Payodhar Padhi

AbstractNanocomposites of Al and Al2O3 were synthesized by an ultrasonic full cavitation technique which is a novel route for synthesis of uniformly distributed nanoparticles in metal matrix composites. The transmission electron micrograph indicates the uniform arrangement of nanoparticles throughout the metal matrix and the average size of the nanoparticles are in the order of 5 nm. The selected area electron diffraction analysis shows the presence of both Al and Al2O3 phases, which is also evidenced from the X-ray photoelectron spectroscopy analysis. The significant improvement in hardness and Young’s modulus due to the addition of a low weight fraction of nano-sized Al2O3 in aluminium infers that alumina nanoparticulates are distributed uniformly throughout the aluminium metal matrix. Hence, this paper shows a new method for inexpensive fabrication of bulk light weight metal matrix nanocomposites (MMNCs) by the use of noncontact full cavitation method.


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