High grain size stability of nanocrystalline Al prepared by mechanical attrition

2001 ◽  
Vol 16 (12) ◽  
pp. 3451-3458 ◽  
Author(s):  
F. Zhou ◽  
J. Lee ◽  
S. Dallek ◽  
E. J. Lavernia

Grain growth in nanocrystalline (nc) Al with a grain size of 26 nm produced by cryogenic mechanical milling was studied through x-ray diffraction, transmission electron microscopy, and differential scanning calorimetry. Grain growth kinetics resembled those of ball-milled nc Fe. For homologous temperatures (T/TM) of 0.51–0.83, the time exponent n from D1/n − D01/n = kt was 0.04–0.28, tending toward 0.5 as T/TM increased. Two grain-growth regimes were distinguished: below T/TM = 0.78 growth ceased at an approximate grain size of 50 nm while at higher temperatures, grain growth proceeded steadily to the submicrometer range. Grain growth over the range of temperatures studied cannot be explained in terms of a single thermally activated rate process. The observed high grain size stability was attributed primarily to impurity pinning drag associated with the grain growth process.

2001 ◽  
Vol 16 (12) ◽  
pp. 3485-3495 ◽  
Author(s):  
Xinghang Zhang ◽  
Haiyan Wang ◽  
Magdy Kassem ◽  
Jagdish Narayan ◽  
Carl C. Koch

Nanocrystalline Zn was prepared by cryomilling (mechanical attrition at liquid nitrogen temperature). Differential scanning calorimetry (DSC), x-ray diffraction, and transmission electron microscopy were used to study the structural changes and grain size distribution with milling time and subsequent annealing. Maxima in both stored enthalpy (for the low-temperature DSC peak) and lattice strain on the Zn basal planes were observed at the same milling time. Dislocation density on the basal planes is proposed as a major source for lattice strain and the measured stored enthalpy. The released enthalpy that might be due to grain growth is very small.


1992 ◽  
Vol 272 ◽  
Author(s):  
J. C. Holzer ◽  
R. Birringer ◽  
J. Eckert ◽  
C.E. Krill ◽  
W.L. Johnson

ABSTRACTNanocrystalline Fe has been prepared by inert gas condensation and ball milling. The kinetics of relaxation and grain growth are investigated by differential scanning calorimetry. The development of the microstructure is monitored by x-ray powder diffraction and transmission electron microscopy. Emphasis is placed on the differences observed for samples prepared by the two different techniques. We find that the kinetics of relaxation and grain growth are very sensitive to the sample preparation method. Samples with the same initial average grain size, as determined by the peak broadening in x-ray diffraction, show very different recovery behavior. The differences are discussed in terms of the estimated grain boundary energies and the initial grain size distribution obtained by the two preparation techniques.


2011 ◽  
Vol 690 ◽  
pp. 234-237 ◽  
Author(s):  
Thangaraju Shanmugasundaram ◽  
Martin Heilmaier ◽  
V. Subramanya Sarma ◽  
B.S Murty

Bulk nanostructured Al-4Cu alloy was synthesized by high energy ball milling followed by vacuum hot pressing. Its thermal stability was investigated up to 450°C using differential scanning calorimetry, X-ray diffraction, and transmission electron microscopy. The results showed that grain growth in this Al-4Cu alloy was very limited and grain sizes in the range of 100 nm were still present in the alloys after exposure to 450 °C corresponding to a temperature as high as 0.77 T/Tm. The TEM investigations reveal that such a high thermal stability against grain growth observed in this alloy is attributed to the presence of ultrafine dispersoids.


1991 ◽  
Vol 225 ◽  
Author(s):  
D. B. Knorr ◽  
K. P. Rodbell ◽  
D. P. Tracy

ABSTRACTPure aluminum films are deposited under a variety of conditions to vary the crystallographic texture. After patterning and annealing at 400°C for 1 hour, electromigration tests are performed at several temperatures. Failure data are compared on the basis of t50 and standard deviation. Microstructure is quantified by transmission electron microscopy for grain size and grain size distribution and by X-ray diffraction for texture. A strong (111) texture significantly improves the electromigration lifetime and decreases the standard deviation in time to failure. This improvement correlates with both the fraction and sharpness of the (111) texture component.


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.


2007 ◽  
Vol 551-552 ◽  
pp. 387-392 ◽  
Author(s):  
Wen Juan Zhao ◽  
Hua Ding ◽  
D. Song ◽  
F.R. Cao ◽  
Hong Liang Hou

In this study, superplastic tensile tests were carried out for Ti-6Al-4V alloy using different initial grain sizes (2.6 μm, 6.5μm and 16.2 μm) at a temperature of 920°C with an initial strain rate of 1×10-3 s-1. To get an insight into the effect of grain size on the superplastic deformation mechanisms, the microstructures of deformed alloy were investigated by using an optical microscope and transmission electron microscope (TEM). The results indicate that there is dramatic difference in the superplastic deformation mode of fine and coarse grained Ti-6Al-4V alloy. Meanwhile, grain growth induced by superplastic deformation has also been clearly observed during deformation process, and the grain growth model including the static and strain induced part during superplastic deformation was utilized to analyze the data of Ti-6Al-4V alloy.


2010 ◽  
Vol 654-656 ◽  
pp. 1106-1109
Author(s):  
Ya Qiong He ◽  
Chang Hui Mao ◽  
Jian Yang

Nanocrystalline Fe-Co alloy powders, which were prepared by high-energy mechanical milling, were nitrided under the mixing gas of NH3/H2 in the temperature range from 380°C to 510°C. X-ray diffraction (XRD) was used to analyze the grain size and reaction during the processing. The magnetic properties of the nitrided powders were measured by Vibrating Sample Magnetometer (VSM). The results show that with the appearance of Fe4N phase after nitride treatment, and the grain-size of FeCo phase decreases with the increase of nitridation temperature between 380°C to 450°C.The saturation magnetization of nitrided alloy powder treated at 480°C is about 18% higher than that of the initial Fe-Co alloy powder, accompanied by the reduction of the coercivity. Transmission electron microscope (TEM) was used, attempting to further analyze the effect of Fe4N phase on microstructure and magnetic properties of the powder mixtures.


1999 ◽  
Vol 580 ◽  
Author(s):  
G.D. Hibbard ◽  
U. Erb ◽  
K.T. Aust ◽  
G. Palumbo

AbstractIn this study, the effect of grain size distribution on the thermal stability of electrodeposited nanocrystalline nickel was investigated by pre-annealing material such that a limited amount of abnormal grain growth was introduced. This work was done in an effort to understand the previously reported, unexpected effect, of increasing thermal stability with decreasing grain size seen in some nanocrystalline systems. Pre-annealing produced a range of grain size distributions in materials with relatively unchanged crystallographic texture and total solute content. Subsequent thermal analysis of the pre-annealed samples by differential scanning calorimetry showed that the activation energy of further grain growth was unchanged from the as-deposited nanocrystalline nickel.


1992 ◽  
Vol 7 (7) ◽  
pp. 1751-1761 ◽  
Author(s):  
J. Eckert ◽  
J.C. Holzer ◽  
C.E. Krill ◽  
W.L. Johnson

Nanocrystalline fcc metals have been synthesized by mechanical attrition. The crystal refinement and the development of the microstructure have been investigated in detail by x-ray diffraction, differential scanning calorimetry, and transmission electron microscopy. The deformation process causes a decrease of the grain size of the fcc metals to 6–22 nm for the different elements. The final grain size scales with the melting point and the bulk modulus of the respective metal: the higher the melting point and the bulk modulus, the smaller the final grain size of the powder. Thus, the ultimate grain size achievable by this technique is determined by the competition between the heavy mechanical deformation introduced during milling and the recovery behavior of the metal. X-ray diffraction and thermal analysis of the nanocrystalline powders reveal that the crystal size refinement is accompanied by an increase in atomic-level strain and in the mechanically stored enthalpy in comparison to the undeformed state. The excess stored enthalpies of 10–40% of the heat of fusion exceed by far the values known for conventional deformation processes. The contributions of the atomic-level strain and the excess enthalpy of the grain boundaries to the stored enthalpies are critically assessed. The kinetics of grain growth in the nanocrystalline fcc metals are investigated by thermal analysis. The activation energy for grain boundary migration is derived from a modified Kissinger analysis, and estimates of the grain boundary enthalpy are given.


2011 ◽  
Vol 479 ◽  
pp. 54-61 ◽  
Author(s):  
Fei Wang ◽  
Ya Ping Wang

Microstructure evolution of high energy milled Al-50wt%Si alloy during heat treatment at different temperature was studied. Scanning electron microscope (SEM) and X-ray diffraction (XRD) results show that the size of the alloy powders decreased with increasing milling time. The observable coarsening of Si particles was not seen below 730°C in the high energy milled alloy, whereas, for the alloy prepared by mixed Al and Si powders, the grain growth occurred at 660°C. The activation energy for the grain growth of Si particles in the high energy milled alloy was determined as about 244 kJ/mol by the differential scanning calorimetry (DSC) data analysis. The size of Si particles in the hot pressed Al-50wt%Si alloy prepared by high energy milled powders was 5-30 m at 700°C, which was significantly reduced compared to that of the original Si powders. Thermal diffusivity of the hot pressed Al-50wt%Si alloy was 55 mm2/s at room temperature which was obtained by laser method.


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