Investigation of the crystallization of ZrO2 (Y2O3 3 mol%) nanopowder

1996 ◽  
Vol 11 (4) ◽  
pp. 917-921 ◽  
Author(s):  
Huiwen Liu ◽  
Qunji Xue

The coprecipitation technique has been used to prepare ZrO2 (Y2O3 3 mol %) nanopowder. The influence of residual NH4Cl and pH value on the crystallization of ZrO2 (Y2O3 3 mol %) nanopowder have been investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), x-ray diffraction (XRD), infrared spectrometry (IR), and transmission electron microscopy (TEM) techniques. The IR spectra proved that the presence of residual NH4Cl increased the amount of the hydroxo group. This led to serious gel agglomerate and free enthalpy decrease. Therefore, the crystallization of ZrO2 (Y2O3 3 mol%) nanopowder is greatly influenced by the residual NH4Cl. While there is no residual NH4Cl, the crystallization takes place at 445 °C and is an exothermic process. On the contrary, with NH4Cl the crystallization takes place at 376 °C and is an endothermic process. However, the pH value does not influence the crystallization of ZrO2 (Y2O3 3 mol%) nanopowder.

Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.


1991 ◽  
Vol 246 ◽  
Author(s):  
J.A. Horton ◽  
E.P. George ◽  
C.J. Sparks ◽  
M.Y. Kao ◽  
O.B. Cavin ◽  
...  

AbstractA survey by differential scanning calorimetry (DSC) and recovery during heating of indentations on a series of nickel-aluminum alloys showed that the Ni-36 at.% Al composition has the best potential for a recoverable shape memory effect at temperatures above 100°C. The phase transformations were studied by high temperature transmission electron microscopy (TEM) and by high temperature x-ray diffraction (HTXRD). Quenching from 1200°C resulted in a single phase, fully martensitic structure. The initial quenched-in martensites were found by both TEM and X-ray diffraction to consist of primarily a body centered tetragonal (bct) phase with some body centered orthorhombic (bco) phase present. On the first heating cycle, DSC showed an endothermic peak at 121°C and an exothermic peak at 289°C, and upon cooling a martensite exothermic peak at 115° C. Upon subsequent cycles the 289°C peak disappeared. High temperature X-ray diffraction, with a heating rate of 2°C/min, showed the expected transformation of bct phase to B2 between 100 and 200°C, however the bco phase remained intact. At 400 to 450°C the B2 phase transformed to Ni2Al and Ni5Al3. During TEM heating experiments a dislocation-free martensite transformed reversibly to B2 at temperatures less than 150°C. At higher temperatures (nearly 600°C) 1/3, 1/3, 1/3 reflections from an ω-like phase formed. Upon cooling, the 1/3, 1/3, 1/3 reflections disappeared and a more complicated martensite resulted. Boron additions suppressed intergranular fracture and, as expected, resulted in no ductility improvements. Boron additions and/or hot extrusion encouraged the formation of a superordered bct structure with 1/2, 1/2, 0 reflections.


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.


2016 ◽  
Vol 5 (5) ◽  
Author(s):  
Phuong Phong Nguyen Thi ◽  
Dai Hai Nguyen

AbstractWe report star-shaped silver@gold (Ag@Au) nanoparticles (NPs) in gelatin suspensions for the purpose of enhancing the stability of Ag@Au NPs. In this case, Ag NPs were designed as nucleating agents, whereas gelatin was used as a protecting agent for Au development. Especially, variable gelatin concentrations were also prepared to explore its ability to increase the stability of Ag@Au NPs. The obtained samples were then characterized by UV-visible spectroscopy, transmission electron spectroscopy (TEM), X-ray diffraction, and Fourier transform infrared spectroscopy. The maximum absorption wavelength of all samples (566–580 nm) indicated that branched Ag@Au@gelatin NPs were successfully synthesized. In addition, our TEM results revealed that the size of branched Ag@Au@gelatin NPs was found to be between 20 and 45 nm as influenced by the component ratio and the pH value. These results can provide valuable insights into the improvement of Ag@Au NP stability in the presence of gelatin.


2012 ◽  
Vol 602-604 ◽  
pp. 227-230
Author(s):  
Tao Fan ◽  
Yan Rong Sun ◽  
Li Guo Ma

Spheroid hydroxyapatite nanoparticles were successfully prepared by titrating Ca(NO3)2•4H2O and (NH4)2HPO4 aqueous solution in the reverse microemulsion, which consists of mixed OP-10(surfactant), cyclohexane(oil phase), and isobutanol (cosurfactant).The structure and morphology of the prepared powders were characterized by means of X-ray diffraction (XRD) and transmission electron microscope (TEM). The optimum composition was investigated via the analysis of the aqueous solution conductivity, and the mechanism of aqueous reaction. The effect of the pH value and the amount of surfactant on the particle size were studied. The results indicate that the best conditions are which the concentration of OP-10 and isobutanol both are 0.2 M, when the water content is between 130 ml-250 ml,it results in pure nano-hydroxyapatite spheroid-like powders, and the water content is about 200 ml, whose diameters are 50 nm-80 nm, and good particle diameter distribution, the particle microstructure is homogeneous, good crystal structure and higher crystallinity.


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.


2012 ◽  
Vol 724 ◽  
pp. 205-208
Author(s):  
Li Yan Zhang ◽  
Fen Wang ◽  
Jian Feng Zhu

ZnO nanorods were prepared by heat treating of aqueous zinc acetate treated with organic of PVA. The products were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscopy (TEM). The results indicate that the as synthesized ZnO are hexagonal wurtzite nanorods with the maximum aspect ratio of 10:1 (100 nm in diameter and about 1 μm in length). The morphology of nanorods was formed by the regulation of appropriate organic under a pH value of 8.5. The growth mechanism of ZnO is proposed that the nanocrystals grow along a preferred direction in a growth tunnel provided by organics.


2008 ◽  
Vol 23 (11) ◽  
pp. 2880-2885 ◽  
Author(s):  
Herbert Willmann ◽  
Paul H. Mayrhofer ◽  
Lars Hultman ◽  
Christian Mitterer

Microstructure and hardness evolution of arc-evaporated single-phase cubic Al0.56Cr0.44N and Al0.68Cr0.32N coatings have been investigated after thermal treatment in Ar atmosphere. Based on a combination of differential scanning calorimetry and x-ray diffraction studies, we can conclude that Al0.56Cr0.44N undergoes only small structural changes without any decomposition for annealing temperatures Ta ⩽ 900 °C. Consequently, the hardness decreases only marginally from the as-deposited value of 30.0 ± 1.1 GPa to 29.4 ± 0.9 GPa with Ta increasing to 900 °C, respectively. The film with higher Al content (Al0.68Cr0.32N) exhibits formation of hexagonal (h) AlN at Ta ⩾ 700 °C, which occurs preferably at grain boundaries as identified by analytical transmission electron microscopy. Hence, the hardness increases from the as-deposited value of 30.1 ± 1.3 GPa to 31.6 ± 1.4 GPa with Ta = 725 °C. At higher temperatures, where the size and volume fraction of the h-AlN phase increases, the hardness decreases to 27.5 ± 1.0 GPa with Ta = 900 °C.


1999 ◽  
Vol 14 (4) ◽  
pp. 1570-1575 ◽  
Author(s):  
G. Ennas ◽  
G. Marongiu ◽  
A. Musinu ◽  
A. Falqui ◽  
P. Ballirano ◽  
...  

Homogeneous maghemite (γ–Fe2O3) nanoparticles with an average crystal size around 5 nm were synthesized by successive hydrolysis, oxidation, and dehydration of tetrapyridino-ferrous chloride. Morphological, thermal, and structural properties were investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) techniques. Rietveld refinement indicated a cubic cell. The superstructure reflections, related to the ordering of cation lattice vacancies, were not detected in the diffraction pattern. Kinetics of the solid-state phase transition of nanocrystalline maghemite to hematite (α–Fe2O3), investigated by energy dispersive x-ray diffraction (EDXRD), indicates that direct transformation from nanocrystalline maghemite to microcrystalline hematite takes place during isothermal treatment at 385 °C. This temperature is lower than that observed both for microcrystalline maghemite and for nanocrystalline maghemite supported on silica.


2006 ◽  
Vol 21 (3) ◽  
pp. 597-607 ◽  
Author(s):  
S. Venkataraman ◽  
S. Scudino ◽  
J. Eckert ◽  
T. Gemming ◽  
C. Mickel ◽  
...  

Cu47Ti33Zr11Ni8Si1 metallic glass powder was prepared by gas atomization. Decomposition in the amorphous alloy and primary crystallization has been studied by differential scanning calorimetry (DSC), x-ray diffraction (XRD), and transmission electron microscopy (TEM). The glassy powder exhibits a broad DSC exotherm prior to bulk crystallization. Controlled annealing experiments reveal that this exotherm corresponds to a combination of structural relaxation and nanocrystallization. A uniform featureless amorphous contrast is observed in the TEM prior to the detection of nanocrystals of 4–6 nm in size. High-resolution TEM studies indicate that this nanocrystalline phase has a close crystallographic relationship with the γ–CuTi phase having a tetragonal structure. The product of the main crystallization event is also nanocrystalline, hexagonal Cu51Zr14, having dimensions of 20 nm. However, there is no evidence for possible amorphous phase separation prior to the nanocrystallization events.


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