Microstructural study of aluminide surface coatings on single crystal nickel base superalloy substrates

Aluminide diffusion coatings are frequently employed to enhance the oxidation resistance of nickel base superalloys. However, there is a concern that the presence of an aluminide coating could influence the properties of the coated superalloy, especially in respect of fatigue behaviour. To understand the nature of the effects of surface coatings on the fatigue properties of superalloys, an understanding of microstructural development within both the coating and the coating/substrate interfacial zone during high temperature fatigue testing is necessary. This paper is concerned with microstructural changes in aluminide diffusion coatings on single crystal γ′ strengthened superalloy substrates during the course of high temperature fatigue testing. The 'edge on' transmission electron microscopy technique is employed to study cross-sections of two stage (aluminization plus diffusion treatment) coated superalloy samples. The paper examines the degradation of the coating produced by phase transformations induced by loss of aluminum from the coating and/or aging of the coating. Aluminum removal both by interdiffusion with the substrate and by oxidation of the coating surface is considered. Microstructural development in the portion of the substrate influenced by interdiffusion with the coating is also discussed.

Decomposition of the B2-type matrix

The microstructural stability of aluminide diffusion coatings, prepared by means of a two-stage pack-aluminization treatment on single-crystal nickel-base superalloy substrates, is considered in this article. Edge-on specimens of coated superalloy are studied using transmission electron microscopy (TEM). The effects of coating thickness and post-coating heat treatment (duration, temperature, and atmosphere) on coating microstructure are examined. The article discusses the partial transformation of the matrix of the coating, from a B2-type phase (nominally NiAl) to a L12 phase (nominally Ni3(Al, Ti)), during exposure at temperatures of 850 °C and 950 °C in air and in vacuum for up to 138 hours. Three possible processes that can account for decom- position of the coating matrix are investigated, namely, interdiffusion between the coating and the substrate, oxidation of the coating surface, and aging of the coating. Of these processes, aging of the coating is shown to be the predominant factor in the coating transformation under the conditions considered. © 1992 The Minerals, Metals and Materials Society, and ASM International.

Microstructural development in aluminide diffusion coatings on nickel-base superalloy single crystals

An investigation has been made of the microstructural stability of aluminide diffusion coatings during post-coating thermal exposure. This study has employed edge-on transmission electron microscopy to examine high-activity pack aluminised single crystals of a gamma prime strengthened nickel-base superalloy. The influence of exposure temperature, duration and atmosphere as well as the initial coating thickness has been assessed. Two major processes have been found to contribute to microstructural changes in the coating. These are, firstly, the transformation of the coating matrix (β-phase, nominally NiAl) to other Ni-Al based phases, especially γ' (nominally Ni3(Al, Ti)) and, secondly, the precipitation of chromium containing phases. The work has enabled the roles of three processes contributing to γ formation, namely: oxidation of the coating surface, interdiffusion with the substrate and ageing of the coating, to be understood. In addition, the factors leading to the formation of a sequence of chromium-containing phases have been identified.

Surface coating deterioration studies

This project is concerned with the deterioration of surface coatings as a result of weathering and exposure to a pollutant gas (in this case nitric oxide). Poly(vinyl chloride) (PVC) plastisol surface coatings have been exposed to natural and artificial weathering and a comparison of the effects of these two types of weathering has been made by use of various analytical techniques. These techniques have each been assessed as to their value in providing information regarding changes taking place in the coatings during ageing, and include, goniophotometry, micro-penetrometry, surface energy measurements, weight loss measurements, thermal analysis and scanning electron microscopy. The results of each of these studies have then been combined to show the changes undergone by PVC plastisol surface coatings during ageing and to show the effects which additives to the coatings have on their behaviour and in particular the effects of plasticiser, pigment and uv and thermal stabilisers. Finally a preliminary study of the interaction between five commercial polymers and nitric oxide has been carried out, the polymers being polypropylene, cellulose acetate butyrate, polystyrene, polyethylene terephthalate and polycarbonate. Each of the samples was examined using infra-red spectroscopy in the transmission mode.

Characterisation and surface-profiling techniques for composite particles produced by dry powder coating in pharmaceutical drug delivery

The production of composite particles using dry powder coating is a one-step, environmentally friendly, process for the fabrication of particles with targeted properties and favourable functionalities. Diverse functionalities, such flowability enhancement, content uniformity, and dissolution, can be developed from dry particle coating. In this review, we discuss the particle functionalities that can be tailored and the selection of characterisation techniques relevant to understanding their molecular basis. We address key features in the powder blend sampling process and explore the relevant characterisation techniques, focussing on the functionality delivered by dry coating and on surface profiling that explores the dynamics and surface characteristics of the composite blends. Dry particle coating is a solvent- and heat-free process that can be used to develop functionalised particles. However, assessment of the resultant functionality requires careful selection of sensitive analytical techniques that can distinguish particle surface changes within nano and/or micrometre ranges.

An ultra-sensitive localised surface plasmon resonance fibre device for environmental sensing based upon a structured bi-metal coating

We demonstrate a bi-metal coating (platinum and gold or silver) localised surface plasmon resonance fibre device that produces an index spectral sensitivity of over 11,000 nm/RIU, yielding an index resolution of 5×10-6in the aqueous index regime, consisting of a structured multi-layered thin film on D-shaped fibre. © 2014 SPIE.

Microparticle surface layering through dry coating:impact of moisture content and process parameters on the properties of orally disintegrating tablets

OBJECTIVES: The aim of this study was to investigate the influence of process parameters during dry coating on particle and dosage form properties upon varying the surface adsorbed moisture of microcrystalline cellulose (MCC), a model filler/binder for orally disintegrating tablets (ODTs). METHODS: The moisture content of MCC was optimised using the spray water method and analysed using thermogravimetric analysis. Microproperty/macroproperty assessment was investigated using atomic force microscopy, nano-indentation, scanning electron microscopy, tablet hardness and disintegration testing. KEY FINDINGS: The results showed that MCC demonstrated its best flowability at a moisture content of 11.2% w/w when compared to control, comprising of 3.9% w/w moisture. The use of the composite powder coating process (without air) resulted in up to 80% increase in tablet hardness, when compared to the control. The study also demonstrated that surface adsorbed moisture can be displaced upon addition of excipients during dry processing circumventing the need for particle drying before tabletting. CONCLUSIONS: It was concluded that MCC with a moisture content of 11% w/w provides a good balance between powder flowability and favourable ODT characteristics.

Use of a solvent-free dry matrix coating for quantitative matrix-assisted laser desorption ionization imaging of 4-bromophenyl-1,4-diazabicyclo(3.2.2)nonane-4-carboxylate in rat brain and quantitative analysis of the drug from laser microdissected tissue regions

A dry matrix application for matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI MSI) was used to profile the distribution of 4-bromophenyl-1,4-diazabicyclo(3.2.2)nonane-4-carboxylate, monohydrochloride (BDNC, SSR180711) in rat brain tissue sections. Matrix application involved applying layers of finely ground dry alpha-cyano-4-hydroxycinnamic acid (CHCA) to the surface of tissue sections thaw mounted onto MALDI targets. It was not possible to detect the drug when applying matrix in a standard aqueous-organic solvent solution. The drug was detected at higher concentrations in specific regions of the brain, particularly the white matter of the cerebellum. Pseudomultiple reaction monitoring imaging was used to validate that the observed distribution was the target compound. The semiquantitative data obtained from signal intensities in the imaging was confirmed by laser microdissection of specific regions of the brain directed by the imaging, followed by hydrophilic interaction chromatography in combination with a quantitative high-resolution mass spectrometry method. This study illustrates that a dry matrix coating is a valuable and complementary matrix application method for analysis of small polar drugs and metabolites that can be used for semiquantitative analysis.

Investigation of liquid sodium alginates as mucoadhesive bandages coating the oesophageal mucosa and protecting it from gastric reflux

Gastro-oesophageal Reflux Disease (GORD), is generally caused by excess gastric reflux back to the oesophagus where damage to the mucosa results in injury. GORD is a very common disease in western countries, more than a quarter of western people are suffering from this disease and there is a trend that the percentage population in eastern countries who are diagnosed as GORD is increasing. GORD and its complications damage the quality of life and can lead to serious oesophageal diseases including Barrett’s disease and oesophageal carcinoma. Sodium alginate dissolved in water forms a viscous liquid and can coat on oesophageal mucosa for a period of time. In this study the ability of the liquid alginate to adhere to the oesophageal mucosa was investigated and the factors that affect this retention were examined. The potential of this liquid alginate as a drug delivery vehicle to extend the duration of contact with the oesophageal mucosa was confirmed by this study. The capacity of an alginate coating to retard acid and pepsin diffusion, the two main aggressive factors in gastric reflux, was investigated. A significant reduction in acid and pepsin diffusion by alginate gel layer was demonstrated in this project, indicating that alginate has great potential to protect against damage caused by acidic reflux. A novel method was introduced using an independent score system to assess the protection of oesophageal tissue by a coating of liquid alginate using microscopy as a technique. This technique demonstrated that alginate can protect the oesophageal epithelial tissue from the damage caused by gastric acid and pepsin. Many techniques were used in this study. The experimental results suggested that liquid sodium alginate is a very promising candidate in treating local oesophageal diseases through forming a coating on the oesophageal mucosal surface, retarding the diffusion of components of gastric refluxate and thus reducing the contact of these noxious factors with the epithelium and minimising injury.

Characterization of infrared surface plasmon resonances generated from a fiber-optical sensor utilizing tilted Bragg gratings

We demonstrate the use of tilted fiber gratings to assist with the generation of infrared surface plasmons on a metal film coating the flat of a D-shaped fiber. The wavelength of the strong (>25 dB) resonance is tunable over similar to 1000 nm by adjusting the polarization state of the light and is highly sensitive to the refractive index of any aqueous medium surrounding the fiber (sensitivity= 3365 nm).

In situ imaging and height reconstruction of phase separation processes in polymer blends during spin coating

Spin coating polymer blend thin films provides a method to produce multiphase functional layers of high uniformity covering large surface areas. Applications for such layers include photovoltaics and light-emitting diodes where performance relies upon the nanoscale phase separation morphology of the spun film. Furthermore, at micrometer scales, phase separation provides a route to produce self-organized structures for templating applications. Understanding the factors that determine the final phase-separated morphology in these systems is consequently an important goal. However, it has to date proved problematic to fully test theoretical models for phase separation during spin coating, due to the high spin speeds, which has limited the spatial resolution of experimental data obtained during the coating process. Without this fundamental understanding, production of optimized micro- and nanoscale structures is hampered. Here, we have employed synchronized stroboscopic illumination together with the high light gathering sensitivity of an electron-multiplying charge-coupled device camera to optically observe structure evolution in such blends during spin coating. Furthermore the use of monochromatic illumination has allowed interference reconstruction of three-dimensional topographies of the spin-coated film as it dries and phase separates with nanometer precision. We have used this new method to directly observe the phase separation process during spinning for a polymer blend (PS-PI) for the first time, providing new insights into the spin-coating process and opening up a route to understand and control phase separation structures. © 2011 American Chemical Society.

Formation and characterization of ultra-sensitive surface plasmon resonance sensor based upon a nano-scale corrugated multi-layered coated D-shaped optical fiber

We present experimental results on the performance of a series of coated, D-shaped optical fiber sensors that display high spectral sensitivities to external refractive index. Sensitivity to the chosen index regime and coupling of the fiber core mode to the surface plasmon resonance (SPR) is enhanced by using specific materials as part of a multi-layered coating. We present strong evidence that this effect is enhanced by post ultraviolet radiation of the lamellar coating that results in the formation of a nano-scale surface relief corrugation structure, which generates an index perturbation within the fiber core that in turn enhances the coupling. We have found reasonable agreement when we modeling the fiber device. It was found that the SPR devices operate in air with high coupling efficiency in excess of 40 dB with spectral sensitivities that outperform a typical long period grating, with one device yielding a wavelength spectral sensitivity of 12000 nm/RIU in the important aqueous index regime. The devices generate SPRs over a very large wavelength range, (visible to 2 mu m) by alternating the polarization state of the illuminating light.

Generation and performance of localised surface plasmons utilising nano-scale structured multi-layered thin films deposited upon D-shaped optical fiber

A new generation of surface plasmonic optical fibre sensors is fabricated using multiple coatings deposited on a lapped section of a single mode fibre. Post-deposition UV laser irradiation using a phase mask produces a nano-scaled surface relief grating structure, resembling nano-wires. The overall length of the individual corrugations is approximately 14 μm with an average full width half maximum of 100 nm. Evidence is presented to show that these surface structures result from material compaction created by the silicon dioxide and germanium layers in the multi-layered coating and the surface topology is capable of supporting localised surface plasmons. The coating compaction induces a strain gradient into the D-shaped optical fibre that generates an asymmetric periodic refractive index profile which enhances the coupling of the light from the core of the fibre to plasmons on the surface of the coating. Experimental data are presented that show changes in spectral characteristics after UV processing and that the performance of the sensors increases from that of their pre-UV irradiation state. The enhanced performance is illustrated with regards to change in external refractive index and demonstrates high spectral sensitivities in gaseous and aqueous index regimes ranging up to 4000 nm/RIU for wavelength and 800 dB/RIU for intensity. The devices generate surface plasmons over a very large wavelength range, (visible to 2 μm) depending on the polarization state of the illuminating light. © 2013 SPIE.