Microstructure Characterization of Ni-75 at.% Al Raney Type Alloy as a Result of Cooling Rate and Chromium Doping

MRS Advances ◽  
2019 ◽  
Vol 4 (25-26) ◽  
pp. 1441-1447
Author(s):  
Naveed Hussain ◽  
Andrew M Mullis ◽  
Jennifer S Forrester

ABSTRACTThe effect of cooling rate on the phase composition of gas atomized Raney type catalysts was studied using the Ni-75 at.% Al composition. The resulting particles were sieved into 3 standard size fractions and analysed using XRD with Rietveld refinement: as expected the three phases, Al₃Ni₂, Al₃Ni, and Al-Al₃Ni eutectic were identified. Differing phase compositions in the 3 size ranges were identified offering a possible explanation for varying catalytic activity with cooling rate, the higher cooling rates experienced by the smaller droplets allow less time for the peritectic conversion of Al₃Ni₂ to Al₃Ni to proceed. This in turn results in a more Al-rich residual liquid, increasing the volume fraction of eutectic. This was further confirmed when analysing the microstructure using SEM backscatter imaging. Al₃Ni₂ was found to be encased in a shell of Al₃Ni characteristic of peritectic reactions. The remainder of the alloy was found to consist of Al-Al₃Ni eutectic. The SEM backscatter imaging also indicated that the larger particles displayed and a more globular structure than smaller particles. Similar Raney type Ni-75 at.% Al doped with 1.5 at.% Cr were synthesised using the same method and sieved into the same 3 standard size fractions. It was found that the Cr doped alloys exhibited a more dendritic character than the undoped samples in the corresponding size fraction, although the material still displayed an increasingly dendritic character with increasing cooling rate. The phase composition found by Rietveld refinement also followed a similar trend to the undoped samples with decreasing amounts of Al₃Ni formed at the higher cooling rates. However, significant amounts of an additional phase, Al₁₃Cr₂, were also observed. Rietveld refinement found that a larger amount of Al₁₃Cr₂ was present than could be accounted for by the addition of 1.5 at.% Cr . This can be explained by the substitution of Ni onto the Cr lattice, as confirmed by Rietveld refinement. Al₁₃Cr₂ was found to be located mostly at the boundary of the Al₃Ni and Al-Al₃Ni eutectic phases during elemental mapping and quantitative image analysis of backscattered electron micrographs. This indicates that precipitation of Al₁₃Cr₂ is towards the end of the solidification process. The relatively large amounts of the Al-rich Al₁₃Cr₂ may explain the enhanced catalytic activity observed following leaching of Cr-doped Raney catalysts.


2013 ◽  
Vol 872 ◽  
pp. 89-93 ◽  
Author(s):  
Nikita Martyushev ◽  
Ilya V. Semenkov ◽  
Yuriy N. Petrenko

The influence of crystallization conditions of leaded tin bronze on the obtained microstructure parameters is examined in the paper. Modification of crystallization conditions was realised by varying the cooling rate of the melt with preheating of the casting molds. Quantitative regularities of the influence of the cooling rate of bronze on its phase composition are presented. Data on mechanical properties of the material under investigation are also reported in the paper. It is demonstrated that high cooling rates (casting into mold at ambient temperature) enable obtaining higher mechanical properties in comparison with low cooling rates (casting into mold heated up to 800 °С).



Author(s):  
Olamilekan R. Oloyede ◽  
Tim Bigg ◽  
Andrew M. Mullis

This study focuses on the fundamental of solidification of commercial grey cast iron as a function of the externally applied cooling rate. Grey cast iron powders were prepared using the drop-tube method, which is a good analogue for commercial production via high pressure gas atomization. The as-solidified droplets were collected and sieved into size ranges from > 850 μm to < 53 μm diameter, with estimated cooling rates of 500 K s−1 to 75,000 K s−1, with each sieve fraction being prepared for metallographic characterization. The microstructure and phase composition of the powders were analyzed using XRD, optical and scanning electron microscopy, with the results being compared against a control sample subject to slow cooling in the drop-tube crucible; which has typical grey cast iron microstructure with extensive flake graphite in a largely ferrite matrix. In contrast, flake graphite was absent in virtually all the drop-tube samples, even in those with the most modest cooling rates. Microstructural analysis revealed that as the cooling rate increased there was less fragmentation of the primary austenite/ferrite dendrites and the volume fraction of primary dendritic material increased. Hence, as the particle fractions get smaller (D < 106 μm) there is a distinct microstructural evidence of a martensite phase which is related to its better mechanical properties (microhardness) as the sample sizes decrease.



2020 ◽  
Vol 21 (2) ◽  
pp. 355-360
Author(s):  
E. V. Sukhova

The structural and phase composition of boron-rich Fe–В–С alloys in the concentration range of 9.0–16.0 % В, 0.001–1.7 % С, Fe – the balance (in wt. %) was investigated in this work. The cooling rate of the alloys was from 10 to 103 К/s. The methods of quantitative metallographic, X-ray, energy dispersive X-ray, and differential thermal analyses were applied. It was established that the maximal solubility of carbon in Fe2B hemiboride does not exceed 0.55 %, and that in FeB monoboride – 0.41 %. The alloys that belong to two-phase peritectic (Fe2(B,C)+Fe(B,C)) region, two-phase peritectic-eutectic (Fe2(B,C)+Fe(B,C)) region, and three-phase peritectic-eutectic (Fe2(B,C)+Fe(B,C)+C) region of the Fe–В–С phase diagram were distinguished depending on their structure. The appearance of an eutectic constituents in the investigated alloys was explained by transition of peritectic reaction L+Fe(В,С)®Fe2(В,С) to eutectic reaction L®Fe(В,С)+Fe2(В,С) within the temperature range of 1623–1583 К in the presence of carbon. With cooling rate increasing from 10 to 103 К/s, structural constituents tended to be fine, their volume fraction changed, microhardness and fracture toughness increased.



2013 ◽  
Vol 813 ◽  
pp. 157-160
Author(s):  
Guang Wei Zhao ◽  
Xi Cong Ye ◽  
Zeng Min Shi ◽  
Wen Jun Liu

The effect of cooling rate on the solicitation microstructure of a ternary cast Al-5.17Cu-2.63Si alloy is investigated. To create widely different cooling rates for the investigated alloy, the melts were cast into four molds made of different materials: aluminum, graphite, sand, and alumina-silicate-fiber felt (a thermal insulated material), respectively. The cooling curves for each mold specimen were simultaneously measured using calibrated K-type thermocouples, which are linked to a PC computer. The microstructures are characterized in terms of eutectic volume fraction and second dendrite arm spacing. The experiment result shows that increasing the cooling rate increases the amount of eutectic phase and decreases significantly the second dendrite arm spacing.



2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Ataallah Bahrami ◽  
Fatemeh Kazemi ◽  
Mirsaleh Mirmohammadi ◽  
Yousef Ghorbani ◽  
Saghar Farajzadeh

AbstractGilsonite has a wide variety of applications in the industry, including the manufacture of electrodes, paints and resins, as well as the production of asphalt and roof-waterproofing material. Gilsonite ash is a determining parameter for its application in some industries (e.g., gilsonite with ash content < 5% used as an additive in drilling fluids, resins). Due to the shortage of high grade (low ash) gilsonite reserves, the aim of this study is to develop a processing flowsheet for the production of ultra-low-ash gilsonite (< 5%), based on process mineralogy studies and processing tests. For this purpose, mineralogical studies and flotation tests have been performed on a sample of gilsonite with an average ash content of 15%. According to mineralogical studies, carbonates and clay minerals are the main associated impurities (more than 90 vol.%). Furthermore, sulfur was observed in two forms of mineral (pyrite and marcasite) and organic in the structure of gilsonite. Most of these impurities are interlocked with gilsonite in size fractions smaller than 105 µm. The size fraction of + 105 − 420 µm has a higher pure gilsonite (approximately 90%) than other size fractions. By specifying the gangue minerals with gilsonite and the manner and extent of their interlocking with gilsonite, + 75 − 420 µm size fraction selected to perform flotation tests. Flotation tests were performed using different reagents including collector (Gas oil, Kerosene and Pine oil), frother (MIBC) and depressant (sodium silicate, tannic acid, sulfuric acid and sodium cyanide) in different dosages. Based on the results, the use of kerosene collector, MIBC frother and a mixture of sodium silicate, tannic acid, sulfuric acid and sodium cyanide depressant had the most favorable results in gilsonite flotation in the rougher stage. Cleaner and recleaner flotation stages for the rougher flotation concentrate resulted in a product with an ash content of 4.89%. Due to the interlocking of gilsonite with impurities in size fractions − 105 µm, it is better to re-grinding the concentrate of the rougher stage beforehand flotation in the cleaner and recleaner stages. Finally, based on the results of mineralogical studies and processing tests, a processing flowsheet including crushing and initial granulation of gilsonite, flotation in rougher, cleaner and recleaner stages has been proposed to produce gilsonite concentrate with < 5% ash content.



2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Guangming Dai ◽  
Lihua Zhan ◽  
Chenglong Guan ◽  
Minghui Huang

Abstract In this study, the differential scanning calorimetry (DSC) tests were performed to measure the nonisothermal crystallization behavior of carbon fiber reinforced polyether ether ketone (CF/PEEK) composites under different cooling rates. The characteristic parameters of crystallization were obtained, and the nonisothermal crystallization model was established. The crystallization temperature range of the material at different cooling rates was predicted by the model. The unidirectional laminates were fabricated at different cooling rates in the crystallization temperature range. The results showed that the crystallization temperature range shifted to a lower temperature with the increase of cooling rate, the established nonisothermal crystallization model was consistent with the DSC test results. It is feasible to shorten the cooling control range from the whole process to the crystallization range. The crystallinity and transverse tensile strength declined significantly with the increase of the cooling rate in the crystallization temperature range. The research results provided theoretical support for the selection of cooling conditions and temperature control range, which could be applied to the thermoforming process of semi-crystalline polymer matrixed composites to improve the manufacturing efficiency.



Crystals ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 72
Author(s):  
Kaushal K. Kesharpu ◽  
Vladislav D. Kochev ◽  
Pavel D. Grigoriev

In highly anisotropic organic superconductor (TMTSF)2ClO4, superconducting (SC) phase coexists with metallic and spin-density wave phases in the form of domains. Using the Maxwell-Garnett approximation (MGA), we calculate the volume ratio and estimate the shape of these embedded SC domains from resistivity data at various temperature and anion disorder, controlled by the cooling rate or annealing time of (TMTSF)2ClO4 samples. We found that the variation of cooling rate and of annealing time affect differently the shape of SC domains. In all cases the SC domains have oblate shape, being the shortest along the interlayer z-axis. This contradicts the widely assumed filamentary superconductivity along the z-axis, used to explain the anisotropic superconductivity onset. We show that anisotropic resistivity drop at the SC onset can be described by the analytical MGA theory with anisotropic background resistance, while the anisotropic Tc can be explained by considering a finite size and flat shape of the samples. Due to a flat/needle sample shape, the probability of percolation via SC domains is the highest along the shortest sample dimension (z-axis), and the lowest along the sample length (x-axis). Our theory can be applied to other heterogeneous superconductors, where the size d of SC domains is much larger than the SC coherence length ξ, e.g., cuprates, iron-based or organic superconductors. It is also applicable when the spin/charge-density wave domains are embedded inside a metallic background, or vice versa.



Nukleonika ◽  
2015 ◽  
Vol 60 (1) ◽  
pp. 29-33
Author(s):  
Mariusz Hasiak

Abstract The microstructure and magnetic properties of nanocomposite hard magnetic Nd-Fe-B-(Re, Ti) materials with different Nd and Fe contents are studied. The role of Re and Ti addition in phase composition and volume fraction of the Nd-Fe-B phase is determined. All samples are annealed at the same temperature of 993 K for 10 min. Mössbauer spectroscopy shows that the addition of 4 at.% of Re to the Nd8Fe78B14 alloy leads to creation of an ineligible amount of the magnetically hard Nd2Fe14B phase. Moreover, the microstructure and magnetic characteristics recorded in a wide range of temperatures for the Nd8Fe79−xB13Mx (x = 4; M = Re or Ti) alloys are also analyzed.



2012 ◽  
Vol 535-537 ◽  
pp. 761-763 ◽  
Author(s):  
Yi Sheng Zhao ◽  
Xin Ming Zhang ◽  
Zhi Guo Gao

The law of phase change of bearing-B steel during continual cooling was studied by adopting dilatometer. The CCT curves of bearing-B steel were drawn, and the effects of RE on critical cooling rates were studied. The experimental results show that the start temperatures of martensite TM was decreased from 438 to 404°C. The critical cooling rate was simultaneously decreased from 33 to 15°C/s.



1994 ◽  
Vol 343 ◽  
Author(s):  
C. M. Scanlan ◽  
M. D. Wiggins ◽  
M. Gajdardziska-Josifovska ◽  
C. R. Aita

ABSTRACTThe mechanical properties of zirconia are known to be a function of phase composition. We show here that a nanolaminate geometry can be used to control the phase composition of zirconia films. The experiment consisted of growth of nanoscale multilayer films (nanolaminates) of polycrystalline zirconia and amorphous alumina by reactive sputter deposition on Si (111) and fused silica substrates. The films were characterized using x-ray diffraction and high resolution electron microscopy. The results show that both monoclinic (m) and tetragonal (t) zirconia polymorphs were formed in the zirconia layers. Most crystallites are oriented with either close-packed {111}-t or {111}-m planes parallel to the substrate. The volume fraction of tetragonal zirconia, the desired phase for transformation-toughening behavior, increases with decreasing zirconia layer thickness. Nanolaminates with a volume fraction of tetragonal zirconia exceeding 0.8 were produced without the addition of a stabilizing dopant, and independent of the kinetic factors that limit tetragonal zirconia growth in pure zirconia films.



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