Amorphous and Crystalline Phase Formation in Ni/Al Multilayer Thin Films

1995 ◽  
Vol 398 ◽  
Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Michaelsen

ABSTRACTWe have investigated reactive phase formation in magnetron sputter-deposited Ni/Al multilayer films with a 1:3 molar ratio and various periodicities ranging from 320 nm to a codeposited film with an effective periodicity of zero. The films were studied by x-ray diffraction, differential scanning calorimetry, electrical resistance measurements, and transmission electron microscopy. We find that a reaction which results in the formation of an amorphous phase has taken place during the multilayer deposition process. This reaction substantially reduces the driving force for subsequent reactions and explains why nucleation kinetics become important for these reactions. The mode of transformation for a film with 10 nm periodicity was investigated, in detail, by applying the Johnson-Mehl-Avrami analysis to data obtained from isothermal and constant heating rate differential scanning calorimetry, in combination with electron microscopy studies of the transformation microstructure.

1997 ◽  
Vol 12 (1) ◽  
pp. 133-146 ◽  
Author(s):  
K. Barmak ◽  
C. Michaelsen ◽  
G. Lucadamo

We have investigated reactive phase formation in magnetron sputter-deposited NiyAl multilayer films with a 1 : 3 molar ratio and various periodicities, L, ranging from 320 nm down to a codeposited film with zero effective periodicity. The films were studied by x-ray diffraction, differential scanning calorimetry, electrical resistance measurements, and transmission electron microscopy. We find that Ni and Al have reacted during deposition to form the B2 NiAl phase and an amorphous phase. The formation of these phases substantially reduces the driving force for subsequent reactions and explains why nucleation kinetics become important for these reactions. Depending on the periodicity, these reactions result in the formation of NiAl3 or Ni2Al9 followed by NiAl3. Detailed calorimetric analysis reveals differences in the nucleation and growth behavior of NiAl3 compared with other studies.


Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Michaelsen

The subject of reactive phase formation in multilayer thin films of varying periodicity has stimulated much research over the past few years. Recent studies have sought to understand the reactions that occur during the annealing of Ni/Al multilayers. Dark field imaging from transmission electron microscopy (TEM) studies in conjunction with in situ x-ray diffraction measurements, and calorimetry experiments (isothermal and constant heating rate), have yielded new insights into the sequence of phases that occur during annealing and the evolution of their microstructure.In this paper we report on reactive phase formation in sputter-deposited lNi:3Al multilayer thin films with a periodicity A (the combined thickness of an aluminum and nickel layer) from 2.5 to 320 nm. A cross-sectional TEM micrograph of an as-deposited film with a periodicity of 10 nm is shown in figure 1. This image shows diffraction contrast from the Ni grains and occasionally from the Al grains in their respective layers.


1993 ◽  
Vol 311 ◽  
Author(s):  
Robert Sinclair ◽  
Toyohiko J. Konno

ABSTRACTWe have studied the reactions at metal-metalloid interfaces using high resolution transmission electron microscopy, including in situ observation, and differential scanning calorimetry. There is contrasting behavior depending on the affinity for interaction or segregation. For reactive systems, compound formation ultimately results, but this can be preceded by solidstate amorphization. For non-reactive systems, crystallization of the metalloid is often achieved with nucleation and growth mediated by the metal phase.


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.


1995 ◽  
Vol 398 ◽  
Author(s):  
K. Barmak ◽  
S. Vivekanand ◽  
F. Ma ◽  
C. Michaelsen

ABSTRACTThe formation of the first phase in the reaction of sputter-deposited Nb/Al multilayer thin films has been studied by power-compensated and heat-flux differential scanning calorimetry, x-ray diffraction and transmission electron microscopy. The modulation periods of the films are in the range of 10-500 nm. Both types of calorimetrie measurements, performed at a constant heating rate, show the presence of two peaks (A and B) for the formation of the single product phase, NbAl3. Isothermal calorimetrie scans show that peak A is associated with a nucleation and growth type transformation. The formation of NbAl3 is thus interpreted as a two-stage process of nucleation and lateral growth to coalescence (peak A) followed by normal growth until the consumption of one or both reactants (peak B). Transmission electron microscopy investigations of samples annealed into the first stage of NbAl3 formation show the presence of this phase at the Nb/Al interface and its preferential growth along the grain boundaries of the Al layer. The latter highlights the role of reactant phase grain structure in product phase formation.


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.


2020 ◽  
Vol 12 (4) ◽  
pp. 22-29
Author(s):  
KanchanV Zade ◽  
Alok Pal Jain

Phytosome is a complex between natural active ingredient and a phospholipid. Further, phytosomes been applied to many popular herbal extracts or active molecules for augmenting oral dissolution. Therefore, in present investigation, orally administered Baicalein, atype of flavanoids, is poorly absorbed, and shows suboptimal dissolution. The phytosomes encapsulating baicalein (1:1 Mm) were prepared by reverse phase evaporation method followed by lyophilization. Transmission electron microscopy (TEM) analysis revealed that phytosomes were almost spherical in shape with particle size below 100 nm. The Powder ex-ray diffraction (PXRD) and differential scanning calorimetry (DSC) demonstrated that Baicalein loaded phytosomes were amorphous in nature. Amorphization of therapeutic moiety leads to improvement in dissolution. In conclusion, epigallocatechin loaded phytosomes exhibited promising results and warrant further in vitro andin vivo investigations under a set of stringent parameters for transforming in to a clinically viable products.


Author(s):  
Xingpu Zhang ◽  
Meng Liu ◽  
Jiangwei Wang ◽  
Jixue Li ◽  
John Banhart

AbstractBoth Sn addition and pre-ageing are known to be effective in maintaining the artificial ageing potential after natural ageing of Al–Mg–Si alloys. In this study, the combined effects of Sn addition and pre-ageing at 100 °C or 180 °C on natural secondary ageing and subsequent artificial ageing of an alloy AA6014 were investigated using hardness, electrical resistivity, differential scanning calorimetry and transmission electron microscopy characterizations. It is found that pre-ageing can suppress natural secondary ageing and improve the artificial ageing hardening kinetics and response after 1 week of natural secondary ageing in both alloys with and without Sn addition. The effect of pre-ageing at 100 °C is more pronounced in the Sn-free alloy while the combination of pre-ageing at 180 °C and adding Sn shows superiority in suppressing natural secondary ageing and thus avoiding the undesired hardening before artificial ageing. Moreover, when natural ageing steps up to 8 h are applied before pre-ageing at 100 °C, the effect of pre-ageing in Sn-added alloy can be further improved. The influence of Sn on vacancies at different ageing temperatures is discussed to explain the observed phenomena. Graphical abstract


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