Synthesis of Al-based metastable alloys by mechanical milling Al and amorphous Fe78Si12B10powders

1994 ◽  
Vol 9 (4) ◽  
pp. 866-874 ◽  
Author(s):  
K. Y. Wang ◽  
A. Q. He ◽  
T. D. Shen ◽  
M. X. Quan ◽  
J. T. Wang

Syntheses of Al-based metastable alloys from powder mixtures of elemental Al and amorphous Fe78Si12B10 [x at. % Al + (100 — x) at. % (Fe78Si12B10)] alloy by mechanical milling (MM) using a planetary ball mill are investigated. X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) are used to characterize their structure during the MM process. For the powder mixture with low content of Al (x = 75, 82), fully amorphous material can be obtained by MM, while for the milled product with a high content of Al (x = 90), nanocrystalline Al and amorphous phases are obtained. During the initial milling stage, the Al atoms are dissolved into the amorphous Fe78Si12B10 matrix by heavy deformation. Consequently, the Al-enriched homogeneous amorphous alloys are produced with the disappearance or shrinkage of diffraction peaks of Al in the XRD pattern. Further milling of the powder mixture with 75 at. % Al results in the crystallization of amorphous phase and the formation of nanocrystalline Al3Fe type phase. The crystallization products of all as-milled samples are very similar, composed of Al13Fe4 and AlFe3 phases. It is suggested that the kinetics of nucleation and growth favor the formation of amorphous phase due to the existence of amorphous phase initially. The amorphization reaction by mechanical milling is diffusion process, but defects and strain also play an important role.

2021 ◽  
Vol 876 ◽  
pp. 7-12
Author(s):  
Petr Urban ◽  
Fátima Ternero Fernández ◽  
Rosa M. Aranda Louvier ◽  
Raquel Astacio López ◽  
Jesus Cintas Físico

The effect of milling time on the microstructure evolution and formation of amorphous phase of Ti60Si40 alloy produced by mechanical alloying (MA) has been investigated. Laser diffraction, Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and Differential Scanning Calorimetry (DSC) were employed to characterize the particle size, morphology and structure of mechanically alloyed Ti60Si40. When the milling time is increased to 20 h, the particle size decreases from 23.7 to 4.7 μm, the shape of the particles changes to spherical and the crystalline structure is transformed into an amorphous phase. The amorphous Ti60Si40 alloy is stable when heating up to 750oC. Above this temperature, the cold crystallization of the intermetallic compounds Ti5Si3 and/or Ti5Si4 begins.


2011 ◽  
Vol 412 ◽  
pp. 263-266
Author(s):  
Hong Wei Zhang ◽  
Li Li Zhang ◽  
Feng Rui Zhai ◽  
Jia Jin Tian ◽  
Can Bang Zhang

The higher mechanical strength of Al87Ce3Ni8.5Mn1.5 nanophase amorphous composites has been obtained with two methods. The first nanophase amorphous composites are directly produced by the single roller spin quenching technology. The method taken for the second nanophase amorphous composites is at first to obtain amorphous single-phase alloy, followed by annealed at different temperatures .The formative condition, the microstructure, the particle size, the volume fraction of α-Al phase and microhardness of nanophase amorphous composites etc have been investigated and compared by X-ray diffraction (XRD) and transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The microstructure of composites produced by the second method is higher than the former, the fabricated material structure of the system is more uniform and the process is easier to control.


2018 ◽  
Vol 32 (8) ◽  
pp. 1078-1091 ◽  
Author(s):  
Sibel Erol Dağ ◽  
Pınar Acar Bozkurt ◽  
Fatma Eroğlu ◽  
Meltem Çelik

A series of polystyrene (PS)/unmodified Na-montmorillonite (Na-MMT) composites were prepared via in situ radical polymerization. The prepared composites were characterized using various techniques. The presence of various functional groups in the unmodified Na-MMT and PS/unmodified Na-MMT composite was confirmed by Fourier transform infrared spectroscopy. Morphology and particle size of prepared composites was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). According to the XRD and TEM results, the interlayer spacing of MMT layers was expanded. SEM images showed a spongy and porous-shaped morphology of composites. TEM revealed the Na-MMT intercalated in PS matrix. The thermal stability of PS/unmodified Na-MMT composites was significantly improved as compared to PS, which is confirmed using thermogravimetric analysis (TGA). The TGA curves indicated that the decomposition temperature of composites is higher at 24–51°C depending on the composition of the mixture than that of pure PS. The differential scanning calorimetry (DSC) results showed that the glass transition temperature of composites was higher as compared to PS. The moisture retention, water uptake, Brunauer–Emmett–Teller specific surface area, and specific pore volume of composites were also investigated. Water resistance of the composites can be greatly improved.


1991 ◽  
Vol 230 ◽  
Author(s):  
Toyohiko J. Konno ◽  
Robert Sinclair

AbstractThe crystallization of amorphous Si in a Al/Si multilayer (with a modulation length of about 120Å) was investigated using transmission electron microscopy, differential scanning calorimetry and X-ray diffraction. Amorphous Si was found to crystallize at about 175 °C with the heat of reaction of 11±2(kJ/mol). Al grains grow prior to the nucleation of crystalline Si. The crystalline Si was found to nucleate within the grown Al layers. The incipient crystalline Si initially grows within the Al layer and then spreads through the amorphous Si and other Al layers. Because of extensive intermixing, the original layered structure is destroyed. The Al(111) texture is also enhanced.


2004 ◽  
Vol 19 (12) ◽  
pp. 3586-3591 ◽  
Author(s):  
Jiyang Chen ◽  
Ying Shi ◽  
Jianlin Shi

Nano-sized (Y,Gd)2O3:Eu powders were synthesized by a novel co-precipitation processing in which a mixture of ammonium hydroxide and ammonium hydrogen carbonate was adopted as a complex precipitant. Evolution behaviors of precursors during calcinations were studied by means of thermogravimetry-differential scanning calorimetry-mass spectrum, Fourier transform infrared, x-ray diffraction, scanning electron microscopy, and transmission electron microscopy in detail. Nano-sized (Y,Gd)2O3:Eu powder as prepared possessed a primary grain size of about 30 nm and specific surface area of 38 m2/g after being calcined at 850 °C for 2 h, showing much finer grains and less agglomeration. The as prepared nanopowder shows intense luminescence at 611nm under x-ray or ultraviolet excitation. Transparent (Y,Gd)2O3:Eu ceramics can also be fabricated using this high sinterable nanopowder.


2009 ◽  
Vol 24 (1) ◽  
pp. 39-49 ◽  
Author(s):  
J. Zhang ◽  
B. Liu ◽  
J.Y. Wang ◽  
Y.C. Zhou

Transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) investigations were conducted on the hot-pressed Ti2SnC bulk ceramic. Microstructure features of bulk Ti2SnC ceramic were characterized by using TEM, and a needle-shaped β-Sn precipitation was observed inside Ti2SnC grains with the orientation relationship: (0001) Ti2SnC // (200) Sn and Ti2SnC // [001] Sn. With the combination of DSC and XRD analyses, the precipitation of metallic Sn was demonstrated to be a thermal stress-induced process during the cooling procedure. The reheating temperature, even as low as 400 °C, could trigger the precipitation of Sn from Ti2SnC, which indicated the low-temperature instability of Ti2SnC. A substoichiometry Ti2SnxC formed after depletion of Sn from ternary Ti2SnC phase. Under electron beam irradiation, metallic Sn was observed diffusing back into Ti2SnxC. Furthermore, a new Ti7SnC6 phase with the lattice constants of a = 0.32 and c = 4.1 nm was identified and added in the Ti-Sn-C ternary system.


2014 ◽  
Vol 21 (1) ◽  
pp. 108-119 ◽  
Author(s):  
Daniela Nunes ◽  
Lídia Santos ◽  
Paulo Duarte ◽  
Ana Pimentel ◽  
Joana V. Pinto ◽  
...  

AbstractThe present work reports a simple and easy wet chemistry synthesis of cuprous oxide (Cu2O) nanospheres at room temperature without surfactants and using different precursors. Structural characterization was carried out by X-ray diffraction, transmission electron microscopy, and scanning electron microscopy coupled with focused ion beam and energy-dispersive X-ray spectroscopy. The optical band gaps were determined from diffuse reflectance spectroscopy. The photoluminescence behavior of the as-synthesized nanospheres showed significant differences depending on the precursors used. The Cu2O nanospheres were constituted by aggregates of nanocrystals, in which an on/off emission behavior of each individual nanocrystal was identified during transmission electron microscopy observations. The thermal behavior of the Cu2O nanospheres was investigated with in situ X-ray diffraction and differential scanning calorimetry experiments. Remarkable structural differences were observed for the nanospheres annealed in air, which turned into hollow spherical structures surrounded by outsized nanocrystals.


2011 ◽  
Vol 172-174 ◽  
pp. 727-732 ◽  
Author(s):  
Ileana Irais Santana ◽  
Francisco Carlos Robles Hernandez ◽  
Vicente Garibay-Febles ◽  
Hector A. Calderon

Composites of Fe-C60and Al C60produced by mechanical milling and sinterized by Spark Plasma Sintering are investigated with special attention to the mechanical properties of the products. The processing involves phase transformations of the fullerenes that are interesting to follow and characterize. This involves formation of tetragonal/rhombohedral diamond and carbides during sintering and milling. Transmission Electron Microscopy (TEM) and Raman Spectroscopy techniques are also used to confirm preliminary results of X Ray Diffraction (XRD) related to the formation of nanostructures i.e., grain size of the crystals during mechanical milling and after sintering, spatial distribution of phases and the different phases that are developed during processing.


2012 ◽  
Vol 730-732 ◽  
pp. 739-744 ◽  
Author(s):  
Petr Urban ◽  
Francisco Gomez Cuevas ◽  
Juan M. Montes ◽  
Jesus Cintas

The amorphization process by mechanical alloying in the Fe-Si alloy system has been studied. High energy ball milling has been applied for alloys synthesis. X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to monitor the structural and phase transformations through the different stages of milling. The addition of amorphous boron in the milling process and the increase of the milling time were used to improve the formation of the amorphous phase. Heating the samples resulted in the crystallization of the synthesized amorphous alloys and the appearance of equilibrium intermetallic compounds.


1992 ◽  
Vol 7 (4) ◽  
pp. 888-893 ◽  
Author(s):  
M. Sherif El-Eskandarany ◽  
K. Sumiyama ◽  
K. Aoki ◽  
K. Suzuki

Nonequilibrium titanium-nitride alloy powders have been fabricated by a high energetic ball mill under nitrogen gas flow at room temperature and characterized by means of x-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Initial hcp titanium is completely transformed to nonequilibrium-fcc Ti–N after 720 ks of the milling time. The fcc Ti–N phase is stable at relatively low temperature and transforms at 855 K to Ti2N and δ phases. At the final stage of milling, the particle- and grain-sizes of alloy powders are 1 mm and 5 nm, respectively, and the lattice parameter is 0.419 nm.


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