AEM-investigation of ceramic coatings on hard metals

Author(s):  
P. Warbichler ◽  
F. Hofer

To improve their working life, hard metal tools are coated with ceramic protective coatings by means of chemical vapour deposition (CVD). Generally, several layers are deposited, e.g. titaniumcarbide, titaniumnitride, titaniumcarbonitride and aluminiumoxide with thicknesses ranging from some 10 nm to some μm.The understanding of mechanical properties of the coatings is dependent on gaining a knowledge of both the interfaces and the structure of the coatings involved. The coating properties are, in turn, dependent on the coating deposition parameters. A detailed understanding of the influence of these parameters on the mechanical and chemical properties of the multilayer/substrate combination is therefore required.The structure and morphology of the multilayer coatings have been already investigated by using optical and scanning electron microscopy (SEM), whereas transmission electron microscopy (TEM) was hitherto only applied to the study of single TiC or Al2O3 coatings.For TEM-investigations cross-sections must be taken through the multilayer coating and the cemented carbide substrate. In our investigations, a method of preparation described by Newcomb et al.

2020 ◽  
Vol 405 ◽  
pp. 33-39
Author(s):  
Elisabeth Rauchenwald ◽  
Mario Lessiak ◽  
Ronald Weissenbacher ◽  
Sabine Schwarz ◽  
Roland Haubner

Chemical vapour deposited HfN can be utilised as a component of multilayer systems in protective coatings on cutting tools. In this study, related AlHfN coatings were synthesized through a reaction of metallic hafnium and aluminium with HCl gas forming gaseous HfCl4 and AlCl3, which were subsequently transported into a heated coating reactor. Via high temperatures and separately introduced NH3 and N2 as reaction gases, AlHfN coatings were deposited on hardmetal inserts. By varying the ratio between AlCl3 and HfCl4, compositionally different AlHfN coatings were examined. Additionally, surface morphology, composition as well as crystalline phases of the obtained coatings were analysed by scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction. Finally, the microstructure of the cross section of a coating was investigated via transmission electron microscopy. The observations revealed a great impact of the gas composition on the morphology and crystal structures of the coatings. Within the layer, the growth of columnar microstructures was detected. Additionally, the formation of an amorphous HfN intermediate layer between the substrate and the AlHfN with a thickness of approximately 2 nm was found.


Author(s):  
Gulzar Ahmed Rather ◽  
Arghya Chakravorty ◽  
Basharat Ahmad Bhat ◽  
Ishfaq Majeed Malik ◽  
Fayaz Hussain Mir ◽  
...  

An interesting aspect of nanotechnology is the remarkable size-dependent physico-chemical properties of nanomaterials that have led to the rise of synthesis procedures for nanomaterials across a range of sizes, shapes, and chemical compositions. This chapter will concentrate on the different methods such as electron irradiation, laser ablation, and chemical reduction, biological methods, photochemical methods; microwave processing, chemical vapour condensation (CVC), arc discharge, hydrogen plasma-metal reaction, and laser pyrolysis in the vapour phase. This chapter will also include the various characterization techniques for the conformation of nanomaterials such as UV-visible spectroscopy, x-ray diffraction, and electron microscopy (e.g., transmission electron microscopy [TEM], scanning electron microscopy [SEM], and atomic force microscopy [AFM]).


Author(s):  
R. W. Anderson ◽  
D. L. Senecal

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.


2010 ◽  
Vol 97-101 ◽  
pp. 4213-4216
Author(s):  
Jian Xiong Liu ◽  
Zheng Yu Wu ◽  
Guo Wen Meng ◽  
Zhao Lin Zhan

Novel single-crystalline SnO2 zigzag nanoribbons have been successfully synthesized by chemical vapour deposition. Sn powder in a ceramic boat covered with Si plates was heated at 1100°C in a flowing argon atmosphere to get deposits on a Si wafers. The main part of deposits is SnO2 zigzag nanoribbons. They were characterized by means of X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). SEM observations reveal that the SnO2 zigzag nanoribbons are almost uniform, with lengths near to several hundred micrometers and have a good periodically tuned microstructure as the same zigzag angle and growth directions. Possible growth mechanism of these zigzag nanoribbons was discussed. A room temperature PL spectrum of the zigzag nanoribbons shows three peaks at 373nm, 421nm and 477nm.The novel zigzag microstructures will provide a new candidate for potential application.


1996 ◽  
Vol 452 ◽  
Author(s):  
U. Klement ◽  
D. Horst ◽  
F. Ernst

AbstractThe objective of this work is to find a material to replace amorphous hydrogenated silicon used as photosensitive part in the “retina” of an “electronic eye”. For that reason, ZnS, ZnSe, CdS and CdSe were chosen for investigations. Thin films, prepared by chemical vapour deposition, were characterized by transmission electron microscopy. The observed microstructures were correlated with the optoelectronic properties of these materials. CdSe was found to be the most promising material for our application. Hence, the influence of a dielectric interlayer and the effects of additional annealing treatments were analyzed for CdSe and will be discussed with respect to the optimization of the material.


1987 ◽  
Vol 1 (2) ◽  
pp. 322-329 ◽  
Author(s):  
H. Warshawsky

The purpose of this paper is to review evidence which casts doubt on the interpretation universally applied to hexagonal images seen in sectioned enamel. The evidence is based on two possible models to explain the hexagonal profiles seen in mammalian enamel with transmission electron microscopy. The "hexagonal ribbon" model proposes that hexagonal profiles are true cross-sections of elongated hexagonal ribbons. The "rectangular ribbon" model proposes that hexagonal profiles are caused by three-dimensional segments that are parallelepipeds contained in the Epon section. Since shadow projections of such rectangular segments give angles that are inconsistent with the hexagonal unit cell, a model based on ribbons with rhomboidal cut ends and angles of 60 and 120° is proposed. The "rhomboidal ribbon" model projects shadows with angles that are predicted by the unit cell. It is suggested that segments of such crystallites in section project as opaque hexagons on the imaging plane in routine transmission electron microscopy. Morphological observations on crystallites in sections - together with predictions from the hexagonal, rectangular, and rhomboidal ribbon models - indicate that crystallites in rat incisor enamel are flat ribbons with rhomboidal cross-sectional shape. Hexagonal images in electron micrographs of thin-sectioned enamel can result from rhomboidal-ended, parallelepiped-shaped segments of these crystallites projected and viewed as two-dimensional shadows.


Sensors ◽  
2020 ◽  
Vol 20 (15) ◽  
pp. 4340
Author(s):  
Han-Wei Chang ◽  
Chia-Wei Su ◽  
Jia-Hao Tian ◽  
Yu-Chen Tsai

Zn-Co-S ball-in-ball hollow sphere (BHS) was successfully prepared by solvothermal sulfurization method. An efficient strategy to synthesize Zn-Co-S BHS consisted of multilevel structures by controlling the ionic exchange reaction was applied to obtain great performance electrode material. Carbon nanotubes (CNTs) as a conductive agent were uniformly introduced with Zn-Co-S BHS to form Zn-Co-S BHS/CNTs and expedited the considerable electrocatalytic behavior toward glucose electro-oxidation in alkaline medium. In this study, characterization with scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) was used for investigating the morphological and physical/chemical properties and further evaluating the feasibility of Zn-Co-S BHS/CNTs in non-enzymatic glucose sensing. Electrochemical methods (cyclic voltammetry (CV) and chronoamperometry (CA)) were performed to investigate the glucose sensing performance of Zn-Co-S BHS/CNTs. The synergistic effect of Faradaic redox couple species of Zn-Co-S BHS and unique conductive network of CNTs exhibited excellent electrochemical catalytic ability towards the glucose electro-oxidation, which revealed linear range from 5 to 100 μM with high sensitivity of 2734.4 μA mM−1 cm−2, excellent detection limit of 2.98 μM, and great selectivity in the presence of dopamine, uric acid, ascorbic acid, and fructose. Thus, Zn-Co-S BHS/CNTs would be expected to be a promising material for non-enzymatic glucose sensing.


Pharmaceutics ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 263 ◽  
Author(s):  
Maria Letizia Manca ◽  
Iris Usach ◽  
José Esteban Peris ◽  
Antonella Ibba ◽  
Germano Orrù ◽  
...  

New three-dimensionally-structured hybrid phospholipid vesicles, able to load clotrimazole in a high amount (10 mg/mL), were obtained for the first time in this work by significantly reducing the amount of water (≤10%), which was replaced with a mixture of glycerol and ethanol (≈90%). A pre-formulation study was carried out to evaluate the effect of both the composition of the hydrating medium and the concentration of the phospholipid on the physico-chemical properties of hybrid vesicles. Four different three-dimensionally-structured hybrid vesicles were selected as ideal systems for the topical application of clotrimazole. An extensive physico-chemical characterization performed using transmission electron microscopy (TEM), cryogenic transmission electron microscopy (cryo-TEM), 31P-NMR, and small-angle X-ray scattering (SAXS) displayed the formation of small, multi-, and unilamellar vesicles very close to each other, and was capable of forming a three-dimensional network, which stabilized the dispersion. Additionally, the dilution of the dispersion with water reduced the interactions between vesicles, leading to the formation of single unilamellar vesicles. The evaluation of the in vitro percutaneous delivery of clotrimazole showed an improved drug deposition in the skin strata provided by the three-dimensionally-structured vesicles with respect to the commercial cream (Canesten®) used as a reference. Hybrid vesicles were highly biocompatible and showed a significant antifungal activity in vitro, greater than the commercial cream Canesten®. The antimycotic efficacy of formulations was confirmed by the reduced proliferation of the yeast cells at the site of infection in vivo. In light of these results, clotrimazole-loaded, three-dimensionally-structured hybrid vesicles appear to be one of the most innovative and promising formulations for the treatment of candidiasis infections.


1990 ◽  
Vol 199 ◽  
Author(s):  
M. Libera ◽  
T. A. Nguyen ◽  
C. Hwang

ABSTRACTA number of techniques for producing TEM cross-sections of thin films have been described in recent years as the need for improved and more-thorough microstructural study of thin-film materials has grown. We have developed a method for producing such cross-sections which involves little sophisticated equipment other than an ion mill for thinning. Following the method of Bravman and Sinclair (J. Elec. Micrs. Tech 1,53–61 (1984)), the film of interest is either deposited on or epoxied to a silicon wafer and a composite of six silicon beams (=3mm × 25mm × 0.5mm) is fabricated. Slices are cut from this composite perpendicular to the film plane, and each slice is mechanically thinned by a series of simple grinding and polishing steps to ∼ 50–100μm. Dimpling is not necessary. The specimen is mounted onto a slotted TEM grid which provides a vehicle for safe handling, and the specimen is ion milled to perforation. We have found the technique to be relatively fast, reliable, and simple. Its success hinges on minimizing the amount of direct handling required when the specimen is thin and fragile. We present a detailed recipe describing its various steps and show typical results from studies of thin films for data-storage applications.


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