Thermally Activated Nucleation and Faceting in Immiscible Cu-Cr thin Films

Author(s):  
K. P. Staudhammer ◽  
L. E. Murr

The use of the electron microscope as an experimental chamber in which nucleation and growth observations can take place simultaneously has allowed in-situ studies to be performed on Cu-Cr thin films. Detailed investigations of the time-temperature sequence of events occurring during phase separation of two immiscible materials have been recorded on motion picture film. Each stage in the process of thermally induced phase separation of these thin films has been examined and characterized.Co-evaporation and deposition of Cu-Cr at ambient temperatures on freshly cleaved (100) NaCI substrates results in a polycrystalline two-component structure such as shown in Fig. I(a) where the average particle size was less than 100A. Microprobe data showed the composition of the co-evaporated film to be 59.4 Cu - 40.6 Cr. The advantage of working with unsupported nucle-ation of films of immiscible materials as compared to other techniques of substrate supported nucleation studies lies in the inherent nature of immiscible materials. Because surface diffusion is a controlling mechanism, nucleation, faceting and subsequent growth are more rapid. Exsolved parti-cles once nucleated are three dimensional with minimal constraints, and are on the surface of the thin film as compared to platelet geometries obtained from nucleation and growth on most substrate-type investigations.

Author(s):  
Thos. E. Hutchinson

Few areas of investigation have benefited more from the use of the electron microscope than thin films. This is most strikingly demonstrated by the state of knowledge of the structure and growth mechanisms prior to and subsequent to electron microscope investigations.The use of the electron microscope as an experimental chamber in which both growth and observation take place simultaneously, has been responsible primarily for the broad quasi-quantitative view of the process of formation of thin films we now hold. The great advantage of the in situ experimental arrangement lies in its ability to examine in detail the time sequence of events occuring during thin film nucleation and growth. Each stage in the process of formation of thin films has been examined, and although questions still remain as to the exact mechanisms involved, the general features are well characterized. These are nucleation of ad-atom clusters on the substrate, growth of the atom clusters both laterally and perpendicular to the substrate, coalescence of the nuclei into larger sub-units and finally, elimination of channels between the extended islands.


Polymers ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 1548
Author(s):  
Peng Zhu ◽  
Huapeng Zhang ◽  
Hongwei Lu

The droplet evaporation effect on the preparation of polyetherimide (PEI) nanoparticles by thermally induced phase separation (TIPS) was studied. PEI nanoparticles were prepared in two routes. In route I, the droplet evaporation process was carried out after TIPS. In route II, the droplet evaporation and TIPS processes were carried out simultaneously. The surface tension and shape parameters of samples were measured via a drop shape analyzer. The Z-average particle diameter of PEI nanoparticles in the PEI/dimethyl sulfoxide solution (DMSO) suspension at different time points was tested by dynamic light scattering, the data from which was used to determine the TIPS time of the PEI/DMSO solution. The natural properties of the products from both routes were studied by optical microscope, scanning electron microscope and transmission electron microscope. The results show that PEI nanoparticles prepared from route II are much smaller and more uniform than that prepared from route I. Circulation flows in the droplet evaporation were indirectly proved to suppress the growth of particles. At 30 °C, PEI solid nanoparticles with 193 nm average particle size, good uniformity, good separation and good roundness were obtained. Route I is less sensitive to temperature than route II. Samples in route I were still the accumulations of micro and nanoparticles until 40 °C instead of 30 °C in route II, although the particle size distribution was not uniform. In addition, a film structure would appear instead of particles when the evaporation temperature exceeds a certain value in both routes. This work will contribute to the preparation of polymer nanoparticles with small and uniform particle size by TIPS process from preformed polymers.


2021 ◽  
Vol 17 (9) ◽  
pp. 1824-1829
Author(s):  
Junlin Li ◽  
Xiangfei Li ◽  
Dong Liang ◽  
Xiaojuan Zhang ◽  
Qing Lin ◽  
...  

This study exploits the potential of zinc oxide nanoparticles (ZnO-NPs) with diverse morphologies as catalysts and antibacterial agent. Spherical ZnO-NPs, rod-shaped ZnO-NPs and flower-shaped ZnO-NPs were prepared by microemulsion method, solvent heat method and hydrothermal method, respectively. The structural characterizations of samples were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. XRD results revealed the formation of spherical ZnO-NPs, rod-shaped ZnO-NPs and flower-shaped ZnO-NPs were all wurtzite crystal structure. SEM results showed that spherical ZnO-NPs had an average particle size of 30–40 nm, rod-shaped ZnO-NPs were about 500 nm long and 100 nm wide with obvious hexagonal crystals. Flower-shaped ZnO-NPs had a three-dimensional appearance with obvious petals. Results of electrochemical HER (Hydrogen evolution reaction) experiments revealed that spherical ZnO-NPs exhibited the highest electrocatalytic activity at the lowest potential voltage due to their largest specific surface area. The antibacterial property of ZnO-NPs samples were studied by the optical density method and disc diffusion method. All samples had antibacterial effects against E. coli. and flower-shaped ZnO-NPs showed the best antibacterial activity due to the largest surface area in comparison with spherical ZnO-NPs and rod-shaped ZnO-NPs, which promised the maximum Zn2+ release as bactericide mechanism that registered in the case of different ZnO-NPs morphologies.


2005 ◽  
Vol 77 (5) ◽  
pp. 815-826 ◽  
Author(s):  
Jaroslav Stejskal ◽  
Irina Sapurina

Several workers from various institutions in six countries have prepared thin films and colloidal polyaniline dispersions. The films were produced in situ on glass supports during the oxidation of anilinium chloride with ammonium peroxydisulfate in water. The average thickness of the films, assessed by optical absorption, was 125 ± 9 nm, and the conductivity of films was 2.6 ± 0.7 S cm–1. Films prepared in 1 mol l–1 HCl had a similar thickness, 109 ± 10 nm, but a higher conductivity, 18.8 ± 7.1 S cm–1. Colloidal polyaniline particles stabilized with a water-soluble polymer, poly(N-vinylpyrrolidone) [poly(1-vinylpyrrolidin-2-one)], have been prepared by dispersion polymerization. The average particle size, 241 ± 50 nm, and polydispersity, 0.26 ± 0.12, have been determined by dynamic light scattering. The preparation of these two supramolecular polyaniline forms was found to be well reproducible.


2011 ◽  
Vol 374-377 ◽  
pp. 1481-1484 ◽  
Author(s):  
Yao Jun Zhang ◽  
Hai Hong Li ◽  
Ya Chao Wang ◽  
De Long Xu

The microstructure and hydration mechanism of alkali-activated fly ash-based geopolymer were studied by means of scanning electron microscope (SEM) coupled with energy dispersive X-ray analysis (EDXA) and field emission scanning electron microscope (FESEM). The FESEM photomicrographs indicted that the fly ash-based geopolymer showed three dimensional frameworks with an average particle size of 50 nm. EDXA results demonstrated that the Na-PSS type geopolymer was produced via the disintegration of Si-O-Al and Si-O-Si chemical bonds and the polycondensation reaction between [SiO4]4-and [AlO4]5- tetrahedrons in spherical fly ash particles under alkaline condition.


2000 ◽  
Vol 14 (22n23) ◽  
pp. 801-808 ◽  
Author(s):  
M. RAJENDRAN ◽  
M. GHANASHYAM KRISHNA ◽  
A. K. BHATTACHARYA

A novel all-inorganic aqueous sol–gel process has been developed to fabricate LaFeO3 thin films by dip-coating. Stable, positively charged colloidal sol particles of hydrous lanthanum ferrite with an average particle size (Z av ) of 7 nm were prepared and coated onto quartz plates under controlled conditions. The sols have been characterized using photon correlation spectroscopy (PCS) for Z av and size distribution. The redispersible gel was characterized by thermogravimetric and differential thermal analysis (TG-DTA) and also by isothermal heating followed by X-ray diffraction to identify the reaction sequence to form LaFeO 3. The sol–gel films as deposited were X-ray amorphous on heating up to 500°C, partially crystalline at 600°C, fully crystalline and single phase at 650°C and above. These films were continuous, polycrystalline, single phase, had uniform thickness in the range between 180 to 1000 nm, depending on deposition conditions, and showed about 80% optical transmittance. The optical band gap varied from 2.7 to 3.3 eV as a function of the annealing temperature. The refractive index increased with increase in annealing temperature from 1.55 at 500°C to 1.86 at 800°C.


1997 ◽  
Vol 12 (12) ◽  
pp. 3260-3265 ◽  
Author(s):  
F. Tcheliebou ◽  
M. Boulouz ◽  
A. Boyer

Thin films of ZrO2 doped with MgO and Gd2O3, 1–1.5 μm in thickness are formed onto nickel substrates by reactive thermal evaporation using a dual-hearth electron gun. X-ray diffraction patterns of the deposits show changes in the crystallographic structure and average particle size as a function of the dopant content. A mixture of monoclinic and tetragonal phases gradually disappears to become a single cubic phase with increasing dopant molar fraction. The average crystallite size deduced from diffraction line broadening decreases as the dopant content increases. This observation is strongly confirmed by scanning electron micrographs which reveal a smooth surface topography. Fine-grained materials obtained here are interpreted in terms of high nucleation rate and kinetically limited grain growth. It appears that composition, crystallographic structure, and microstructure relations are of paramount importance in ZrO2-based films prepared by electron-beam evaporation.


2008 ◽  
Vol 8 (8) ◽  
pp. 4068-4072 ◽  
Author(s):  
P. B. Patil ◽  
S. Rout ◽  
A. R. B. Rao ◽  
M. Senthil Kumar

Structural and magnetotransport properties of metallic FexAgyAlz nanogranular thin films were studied. These films with several compositions were prepared by dc magnetron sputtering. X-ray diffraction (XRD) measurements carried out on the samples show only Ag(111) peaks. The d-spacings determined from the Ag(111) peaks are smaller than the standard value for bulk Ag indicating a partial substitution of Fe and Al atoms in Ag matrix. Transmission electron diffraction (TEM) patterns show a number of Ag rings. Both XRD and TEM studies did not reveal any diffraction peaks due to Fe or Al. The average particle size determined from the TEM micrograph is 5.9 nm. This value is in good agreement with the grain size determined from the XRD patterns for the Al substituted samples. The MR was found to increase for smaller Al concentration and it decreases with further increase in Al content. In the samples investigated magnetoresistance ratio reaches a maximum value of about 4.5% for the Fe27 Ag63Al10 film.


2018 ◽  
Vol 12 (1) ◽  
pp. 36-44 ◽  
Author(s):  
Abbas Sadeghzadeh-Attar ◽  
Saeid Hajijafari-Bidgoli ◽  
Mohammad Bafandeh

Bismuth silicate (Bi4Si3O12, BSO) nanostructured films containing 0,1,2, and 3mol% Sr were prepared via sol-gel method and annealed at different temperatures up to 700?C. The effects of Sr content on the structure and morphology of prepared films were investigated. SEM images showed that surfaces of the prepared films were dense, smooth and homogeneous. The average particle size was changed from 30 to 35 nm as the annealing temperature was increased from 500 to 700?C. Variation of the dielectric constant and dielectric loss as a function of frequency and annealing temperature for the synthesized thin films with different content of Sr were also studied. The dielectric constant and dielectric loss decrease with Sr addition, and reach the minimum for the sample containing 2mol% Sr. These changes could be attributed to the crystal structure and formation of secondary phases.


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